A method for producing Fmoc-O-tert-butyl-L-glutamic acid

Abstract

A method for producing Fmoc-O-tert-butyl-L-glutamic acid includes the following steps: S1: N-fluorenylmethoxycarbonyl-L-glutamic acid (Fmoc-Glu), potassium carbonate, tert-butyl chloride, and dichloromethane are added sequentially to a reaction vessel. Nitrogen gas is then introduced into the reaction vessel, and the reaction is carried out under nitrogen protection by stirring at room temperature; S2: After the reaction is completed, the reactants are removed from the reaction vessel, and an appropriate amount of water is added to extract the organic phase. The organic phase is then washed with saturated brine; S3: After washing, the organic phase is dried with anhydrous sodium sulfate, filtered to remove sodium sulfate, and dichloromethane is recovered by vacuum distillation to obtain a crude product; S4: The crude product is dissolved in ethyl acetate, and the insoluble matter is removed by filtration. The ethyl acetate is then recovered by vacuum distillation to obtain Fmoc-O-tert-butyl-L-glutamic acid.

Description

Technical Field

[0001] This invention relates to the field of pharmaceutical synthesis and production technology, specifically to a method for producing Fmoc-O-tert-butyl-L-glutamic acid. Background Technology

[0002] In the production of Fmoc-O-tert-butyl-L-glutamic acid, N-fluorenylmethoxycarbonyl-L-glutamic acid (Fmoc-Glu), potassium carbonate, tert-butyl chloride, and dichloromethane are placed in a reaction vessel and stirred to allow them to react. During this reaction, in order to prevent substances in the air from affecting the reaction, the air is usually evacuated before stirring and then nitrogen is introduced for protection. However, if the operator does not notice in time to stop the nitrogen introduction when the existing reaction vessel is filled with nitrogen, the reaction vessel may explode due to excessive nitrogen introduction. Summary of the Invention

[0003] (1) Technical problems to be solved

[0004] The purpose of this invention is to overcome the shortcomings of the prior art, adapt to practical needs, and provide a method for producing Fmoc-O-tert-butyl-L-glutamic acid that avoids the explosion of the reaction vessel caused by the operator's failure to detect and stop nitrogen charging in time, so as to solve the above-mentioned technical problems.

[0005] (2) Technical solution

[0006] To achieve the objectives of this invention, the technical solution adopted is as follows:

[0007] A method for producing Fmoc-O-tert-butyl-L-glutamic acid includes the following steps:

[0008] S1: N-fluorenylmethoxycarbonyl-L-glutamic acid (Fmoc-Glu), potassium carbonate, tert-butyl chloride and dichloromethane are added sequentially to the reaction vessel. Then nitrogen gas is introduced into the reaction vessel. Under the protection of nitrogen gas introduced into the reaction vessel, the reaction is carried out by stirring at room temperature.

[0009] S2: After the reaction is complete, remove the reactants from the reaction vessel, add an appropriate amount of water, extract the organic phase, and wash the organic phase with saturated brine.

[0010] S3: After washing, the organic phase is dried with anhydrous sodium sulfate, the sodium sulfate is removed by filtration, and the dichloromethane is recovered by vacuum distillation to obtain the crude product.

[0011] S4: The crude product was dissolved in ethyl acetate, filtered to remove insoluble matter, and then the ethyl acetate was recovered by vacuum distillation to obtain Fmoc-O-tert-butyl-L-glutamic acid.

[0012] The reaction vessel in step S1 includes a base, a vessel body fixedly mounted on the top surface of the base, an electric motor fixedly mounted on the base, a first connecting hole connected to the vessel body on the bottom surface of the vessel body, a rotating shaft fixedly mounted on the output end of the electric motor, the rotating shaft being able to rotate within the first connecting hole, and the outer peripheral wall of the rotating shaft always maintaining a seal with the inner peripheral wall of the first connecting hole, multiple stirring blades fixedly mounted on the rotating shaft, a feed inlet on the top surface of the vessel body, an electric sliding door for closing the feed inlet on the top surface of the vessel body, a second connecting hole on the electric sliding door, an electric ball valve fixedly mounted on the second connecting hole, a pressure sensor for detecting the gas pressure inside the vessel body on the electric sliding door, a vacuum pump mounted on one side of the vessel body, a first outlet pipe connected between the inlet of the vacuum pump and the vessel body, a second outlet pipe connected between the outlet of the vacuum pump and an external waste gas storage tank, and a nitrogen filling device mounted on the vessel body.

[0013] The nitrogen filling device includes a first air pump placed on one side of the tank, a second air pump placed above the first air pump, a third connecting hole connected to the inside of the tank on the top surface of the tank, a first vent pipe connected to the third connecting hole, the other end of the first vent pipe connected to the outlet of the first air pump, a second vent pipe connected to the inlet of the first air pump, the second vent pipe connected to an external nitrogen storage tank, a third vent pipe connected to the inlet of the second air pump, the third vent pipe connected to the first vent pipe, and a fourth vent pipe connected to the outlet of the second air pump, the fourth vent pipe connected to an external nitrogen storage tank. The first air pump is used to fill the tank with nitrogen from the external nitrogen storage tank, and the second air pump is used to fill the tank with nitrogen back into the external nitrogen storage tank.

[0014] A triggering device is installed inside the tank, and a working device that cooperates with the triggering device is installed above the triggering device.

[0015] The triggering device includes an installation tube fixedly installed on the top wall of the tank body, a pressure plate that can reciprocate in a sealable manner is installed inside the installation tube, and a support spring is fixedly installed between the pressure plate and the top wall of the tank body.

[0016] The working device includes a through hole in the top wall of the tank body, a reciprocating linkage rod that can be sealed within the through hole, a fifth venting steel pipe connected to the first venting steel pipe, the other end of the fifth venting steel pipe being connected to an external nitrogen storage tank, a connecting plate fixedly mounted on the top of the linkage rod, a mating block fixedly mounted on the connecting plate, a spiral groove provided in the mating block, a spiral rod provided in the spiral groove, a rotating shaft fixedly mounted at the upper end of the spiral rod, a working circular hole communicating with the inside of the fifth venting steel pipe provided on the side of the fifth venting steel pipe, the rotating shaft being able to rotate within the working circular hole, and the outer peripheral wall of the rotating shaft always maintaining a seal with the inner peripheral wall of the working circular hole, a working disc fixedly mounted on the side of the rotating shaft for blocking the communication inside the fifth venting steel pipe.

[0017] A positioning plate is fixedly installed on the side of the fifth vent steel pipe, and a positioning groove is provided on the positioning plate. A slider that can reciprocate within the positioning groove is fixedly installed on the connecting plate.

[0018] The first venting steel pipe is provided with a reciprocating push plate. A baffle plate is fixedly provided on the bottom surface of the push plate. A first flow hole is provided in the middle of the push plate. A second flow hole and a sealing gasket are provided on the baffle plate, and the second flow hole is located above the sealing gasket.

[0019] The outer peripheral wall of the working disc is fixedly provided with a first sealing ring, and the inner peripheral wall of the fifth venting steel pipe is fixedly provided with a second sealing ring for cooperating with the first sealing ring.

[0020] A stroke groove is provided on each side of the inner wall of the first venting steel pipe. A stroke block that can reciprocate within the stroke groove is fixedly provided on each side of the push plate. A return spring is fixedly provided between the stroke block and the inner wall of the stroke groove.

[0021] Beneficial effects

[0022] A. By setting up a pressure sensor, the pressure inside tank 2 can be observed through the pressure value displayed on the pressure sensor, so that the operator can turn off the first air pump 100 in time after filling with nitrogen to stop filling with nitrogen, thereby avoiding an explosion inside tank 2.

[0023] B. If the operator fails to see the pressure value of the pressure sensor reach the preset value in time or the pressure value displayed on the pressure sensor is incorrect, resulting in the failure to shut off the air pump in time to allow nitrogen to continue filling the tank 2, there is a risk of explosion. However, by using the triggering device and working device set above, the risk of explosion caused by the operator failing to see the pressure value of the pressure sensor reach the preset value or the pressure value displayed on the pressure sensor being incorrect can be effectively avoided.

[0024] C. After the reaction is complete, start the second gas pump to draw the nitrogen in the tank back into the nitrogen storage tank. The second flow hole and sealing gasket ensure that when nitrogen is being filled from the nitrogen storage tank into the reaction tank, the second flow hole is aligned with the fifth vent pipe, connecting the fifth vent pipe to the first vent pipe. This allows nitrogen to flow back into the nitrogen storage tank through the fifth vent pipe when the reaction tank is full, preventing the reaction tank from exploding. Simultaneously, when nitrogen is being drawn back from the reaction tank into the nitrogen storage tank, the lack of nitrogen flowing downwards to push the baffle plate is a significant safety feature. The second flow hole is aligned with the fifth vent pipe, and the sealing gasket is aligned with the fifth vent pipe, thus blocking the fifth vent pipe from the first vent pipe. This prevents the second air pump from simultaneously drawing nitrogen from the tank and also drawing nitrogen from the nitrogen storage tank due to the connection between the fifth and first vent pipes, which would slow down the efficiency of the second air pump in absorbing nitrogen from the tank. This arrangement allows the second air pump to more quickly draw nitrogen back into the nitrogen storage tank, thereby improving efficiency. Furthermore, by drawing back nitrogen, it can be recycled, thus saving energy. Attached Figure Description

[0025] Figure 1 This is a schematic diagram of the internal mechanism of the present invention;

[0026] Figure 2 for Figure 1 Enlarged view of point A in the image;

[0027] Figure 3 for Figure 2 Enlarged view of point B in the image;

[0028] Figure 4 for Figure 2 Enlarged view of point C in the image;

[0029] Figure 5 for Figure 4 Enlarged view of point D in the image;

[0030] Figure 6 This is a schematic diagram showing the position between the push plate and the first vent steel pipe;

[0031] Figure 7 This is a schematic diagram showing the position between the working disc and the fifth vent pipe.

[0032] Figure 8 for Figure 7 Enlarged view of point E in the image. Detailed Implementation

[0033] The following is in conjunction with the appendix Figure 1-8 The present invention is further illustrated by the embodiments:

[0034] A method for producing Fmoc-O-tert-butyl-L-glutamic acid (the chemical formula of Fmoc-O-tert-butyl-L-glutamic acid is C24H27NO6) includes the following steps:

[0035] S1: Add N-fluorenylmethoxycarbonyl-L-glutamic acid (Fmoc-Glu), potassium carbonate, tert-butyl chloride and dichloromethane sequentially to the reaction vessel, then purge the reaction vessel with nitrogen gas, and allow the reaction to occur by stirring at room temperature under nitrogen protection.

[0036] S2: After the reaction is complete, remove the reactants from the reaction vessel, add an appropriate amount of water, extract the organic phase, and wash the organic phase with saturated brine.

[0037] S3: After washing, the organic phase is dried with anhydrous sodium sulfate, the sodium sulfate is removed by filtration, and the dichloromethane is recovered by vacuum distillation to obtain the crude product.

[0038] S4: The crude product is dissolved in ethyl acetate, filtered to remove insoluble matter, and then ethyl acetate is recovered by vacuum distillation to obtain Fmoc-O-tert-butyl-L-glutamic acid; (Vacuum distillation can reduce the system pressure and lower the boiling point, making the boiling point difference between ethyl acetate and other substances greater, thereby achieving more effective separation.)

[0039] The reaction vessel in step S1 includes a base 1, a vessel body 2 fixedly mounted on the top surface of the base 1, a motor 3 fixedly mounted on the base 1, a first connecting hole 4 communicating with the inside of the vessel body 2 on the bottom surface of the vessel body 2, a rotating shaft 5 fixedly mounted on the output end of the motor 3, the rotating shaft 5 being able to rotate within the first connecting hole 4, and the outer peripheral wall of the rotating shaft 5 always maintaining a seal with the inner peripheral wall of the first connecting hole 4, a plurality of stirring blades 6 fixedly mounted on the rotating shaft 5, a feed inlet 7 on the top surface of the vessel body 2, and an electric sliding door 8 for closing the feed inlet 7 on the top surface of the vessel body 2, the electric sliding door 8 being provided with a second connecting hole. An electric ball valve 10 is fixedly installed on the second connecting hole 9. An electric sliding door 8 is equipped with a pressure sensor that can detect the pressure inside the tank 2 (the pressure inside the tank 2 can be observed by the pressure value displayed on the pressure sensor, so that the operator can shut off the first air pump 100 in time to stop the nitrogen filling after filling). A vacuum pump 233 is installed on one side of the tank 2. A first air outlet pipe 234 is connected between the air inlet of the vacuum pump 233 and the tank 2. A second air outlet pipe 235 is connected between the air outlet of the vacuum pump 233 and the external waste gas storage box. A nitrogen filling device is installed on the tank 2.

[0040] The nitrogen filling device includes a first air pump 100 placed on one side of the tank 2, a second air pump 101 placed above the first air pump 100, a third connecting hole 102 on the top surface of the tank 2 communicating with the inside of the tank 2, a first vent pipe 103 connected to the third connecting hole 102, the other end of the first vent pipe 103 connected to the outlet of the first air pump 100, and a second vent pipe 104 connected to the inlet of the first air pump 100, the second vent pipe 104 being connected to the outside. The first air pump 100 is connected to the nitrogen storage tank. The inlet end of the second air pump 101 is connected to the third vent steel pipe 105, which is connected to the first vent steel pipe 103. The outlet end of the second air pump 101 is connected to the fourth vent steel pipe 106, which is connected to the external nitrogen storage tank. The first air pump 100 is used to fill the tank body 2 with nitrogen from the external nitrogen storage tank. The second air pump 101 is used to fill the tank body 2 with nitrogen back into the external nitrogen storage tank.

[0041] A triggering device is installed inside the tank body 2, and a working device that cooperates with the triggering device is installed above the triggering device.

[0042] The triggering device includes an installation tube 400 fixedly installed on the inner top wall of the tank body 2. A pressure plate 401 that can reciprocate in a sealable manner is provided inside the installation tube 400. A support spring 402 is fixedly installed between the pressure plate 401 and the inner top wall of the tank body 2.

[0043] The working device includes a through hole 500 disposed on the top wall of the tank body 2. A reciprocating linkage rod 501 capable of sealing reciprocation is disposed within the through hole 500. A fifth venting steel pipe 502 is connected to the first venting steel pipe 103. The other end of the fifth venting steel pipe 502 is connected to an external nitrogen storage tank. A connecting plate 503 is fixedly disposed on the top of the linkage rod 501. A mating block 504 is fixedly disposed on the connecting plate 503. A spiral groove 505 is disposed within the mating block 504. A spiral rod 506 is provided inside the groove 505. A rotating shaft 507 is fixedly provided at the upper end of the spiral rod 506. A working circular hole 508 communicating with the inside of the fifth vent steel pipe 502 is provided on the side of the fifth vent steel pipe 502. The rotating shaft 508 can rotate within the working circular hole 508, and the outer peripheral wall of the rotating shaft 508 and the inner peripheral wall of the working circular hole 508 are always sealed. A working disc 510 for blocking the communication inside the fifth vent steel pipe 502 is fixedly provided on the side of the rotating shaft 507.

[0044] A positioning plate 600 is fixedly installed on the side of the fifth ventilation steel pipe 502. A positioning groove 601 is provided on the positioning plate 600. A slider 602 that can reciprocate within the positioning groove 601 is fixedly installed on the connecting plate 503.

[0045] The first ventilation steel pipe 103 is provided with a reciprocating push plate 700. A baffle plate 701 is fixedly provided on the bottom surface of the push plate 700. A first flow hole 702 is provided in the middle of the push plate 700. A second flow hole 703 and a sealing gasket 704 are provided on the baffle plate 701, and the second flow hole 703 is located above the sealing gasket 704.

[0046] The outer peripheral wall of the working disk 510 is fixedly provided with a first sealing ring 610, and the inner peripheral wall of the fifth vent steel pipe 502 is fixedly provided with a second sealing ring 611 for cooperating with the first sealing ring 610.

[0047] The first ventilation steel pipe 103 has a stroke groove 800 on each side of its inner wall. The push plate 700 has a stroke block 801 fixedly installed on each side of its inner wall. The stroke block 801 can reciprocate within the stroke groove 800. A return spring 802 is fixedly installed between the stroke block 801 and the inner wall of the stroke groove 800.

[0048] The working principle of this invention is as follows: Open the electric sliding door 8 to allow N-fluorenemethyloxycarbonyl-L-glutamic acid (Fmoc-Glu), potassium carbonate, tert-butyl chloride, and dichloromethane to be introduced into the tank 2 through the inlet 7. Then, close the inlet 7 using the electric sliding door 8. Start the vacuum pump 233 to allow air from the tank 2 to enter the external waste gas storage tank through the first outlet pipe 234, the vacuum pump 233, and the second outlet pipe 235. Start the first air pump 100 to allow nitrogen from the external nitrogen storage tank to pass through the second outlet pipe 235. Ventilation pipe 104, first air pump 100, and first ventilation pipe 103 enter tank 2 (at this time, second air pump 101 is closed, blocking the third ventilation pipe 105, so nitrogen only flows to first ventilation pipe 103). When the injected nitrogen enters tank 2 through first ventilation pipe 103, it passes through first flow hole 702. Simultaneously, the thrust of the injected nitrogen pushes push plate 700 downward to press return spring 802, causing second flow hole 703 to move accordingly. Plate 700 moves downward, connecting the second flow hole 703 to the fifth vent steel pipe 502. When too much nitrogen is filled into the tank 2, causing the gas pressure inside the tank 2 to exceed the preset value, the gas pressure inside the tank 2 will push the pressure plate 401 to move upward against the resistance of the support spring 402. The upward movement of the pressure plate 401 will also move the linkage rod 501, the connecting plate 503, and the mating block 504 upward together. When the mating block 504 moves upward, the engagement of the spiral groove 505 and the spiral rod 506 will cause the spiral to move upward. The rod 506 rotates, and the rotation of the spiral rod 506 will drive the working disc 510 to rotate 90° counterclockwise, so that the working disc 510 no longer blocks the fifth vent steel pipe 502. This allows the nitrogen gas that is filled into the first vent steel pipe 103 to enter the fifth vent steel pipe 502 through the second flow hole 703 when it passes through the second flow hole 703, and then return to the nitrogen storage tank. This can prevent the tank 2 from being filled with too much nitrogen and exploding because the nitrogen is not stopped in time when the tank 2 is full.

[0049] An explosion may occur if the operator fails to notice that the pressure value of the pressure sensor has reached the preset value or if the pressure value displayed on the pressure sensor is incorrect, thus failing to shut off the air pump in time to allow nitrogen to continue filling the tank 2. However, the above-mentioned triggering device and working device can effectively prevent an explosion caused by the operator failing to notice that the pressure value of the pressure sensor has reached the preset value or if the pressure value displayed on the pressure sensor is incorrect.

[0050] Once the reaction vessel is filled with nitrogen, the first gas pump 100 is shut off (at this time, the push plate 700 and the second flow hole 703 will return to their original position under the action of the return spring 802 after losing the thrust of nitrogen, allowing the sealing gasket 704 to block the fifth vent steel pipe 502 again). Then, the motor 3 is started, and the motor 3 drives the rotating shaft 5 and multiple stirring blades 6 to rotate, stirring the material in the tank 2 to cause a reaction.

[0051] After the reaction is complete, the second gas pump 101 is activated to draw the nitrogen gas in tank 2 back into the nitrogen storage tank. The second flow hole 703 and the sealing gasket 704 ensure that when nitrogen gas is being filled from the nitrogen storage tank into the reaction tank, the second flow hole 703 is aligned with the fifth vent pipe 502, connecting the fifth vent pipe 502 to the first vent pipe 103. This allows nitrogen gas to flow back from the fifth vent pipe 502 into the nitrogen storage tank when the reaction tank is full, preventing the reaction tank from exploding. Simultaneously, when nitrogen gas is being drawn back from the reaction tank into the nitrogen storage tank, the lack of downward pressure from nitrogen gas pushes the baffle plate 700 downwards, allowing the second flow hole to flow back into the nitrogen storage tank. Hole 703 faces the fifth vent steel pipe 502, and therefore the sealing gasket 704 faces the fifth vent steel pipe 502, blocking the fifth vent steel pipe 502 from the first vent steel pipe 103. This prevents the second air pump 101 from drawing nitrogen from the tank 2 while simultaneously drawing nitrogen from the nitrogen storage tank due to the connection between the fifth vent steel pipe 502 and the first vent steel pipe 103, thus slowing down the working efficiency of the second air pump 101 in absorbing nitrogen from the tank 2. This arrangement allows the second air pump 101 to more quickly draw nitrogen from the tank 2 back into the nitrogen storage tank, thereby improving working efficiency. Furthermore, by drawing back nitrogen, nitrogen can be recycled, thus saving energy.

[0052] After the nitrogen gas in tank 2 is evacuated, under the downward reset action of the support spring 402, the pressure plate 401, along with the linkage rod 501, the rotating shaft 507, and the working disc 510, will reset together. That is, the working disc 510 will return to the state of blocking the fifth vent pipe 502. Figure 7 As shown.

[0053] The nitrogen storage tank connected to the outside world by the second venting steel pipe 104, the fourth venting steel pipe 106, and the fifth venting steel pipe 502 is the same nitrogen storage tank.

[0054] The embodiments disclosed herein are preferred embodiments, but are not limited thereto. Those skilled in the art can readily grasp the spirit of the present invention based on the above embodiments and make different extensions and variations, but as long as they do not depart from the spirit of the present invention, they are all within the protection scope of the present invention.

Claims

1. A method for producing Fmoc-O-tert-butyl-L-glutamic acid, characterized in that: Includes the following steps: S1: Add N-fluorenylmethoxycarbonyl-L-glutamic acid (Fmoc-Glu), potassium carbonate, tert-butyl chloride and dichloromethane sequentially to the reaction vessel, then purge the reaction vessel with nitrogen gas, and allow the reaction to occur by stirring at room temperature under nitrogen protection. S2: After the reaction is complete, remove the reactants from the reaction vessel, add an appropriate amount of water, extract the organic phase, and wash the organic phase with saturated brine. S3: After washing, the organic phase is dried with anhydrous sodium sulfate, the sodium sulfate is removed by filtration, and the dichloromethane is recovered by vacuum distillation to obtain the crude product. S4: The crude product was dissolved in ethyl acetate, filtered to remove insoluble matter, and then the ethyl acetate was recovered by vacuum distillation to obtain Fmoc-O-tert-butyl-L-glutamic acid. The reaction vessel in step S1 includes a base (1), a vessel body (2) is fixedly mounted on the top surface of the base (1), an electric motor (3) is fixedly mounted on the base (1), a first connecting hole (4) is provided on the bottom surface of the vessel body (2) and communicates with the inside of the vessel body (2), a rotating shaft (5) is fixedly mounted on the output end of the electric motor (3), the rotating shaft (5) can rotate in the first connecting hole (4), and the outer peripheral wall of the rotating shaft (5) and the inner peripheral wall of the first connecting hole (4) are always sealed, a plurality of stirring blades (6) are fixedly mounted on the rotating shaft (5), and a feed inlet (7) is provided on the top surface of the vessel body (2) for feeding the material. An electric sliding door (8) is used to close the opening (7). The electric sliding door (8) is provided with a second connecting hole (9). An electric ball valve (10) is fixedly installed on the second connecting hole (9). An air pressure sensor that can detect the air pressure inside the tank (2) is provided on the electric sliding door (8). A vacuum pump (233) is provided on one side of the tank (2). A first air outlet pipe (234) is provided between the air inlet of the vacuum pump (233) and the tank (2). A second air outlet pipe (235) is provided between the air outlet of the vacuum pump (233) and the exhaust gas storage box outside. A nitrogen filling device is provided on the tank (2). A triggering device is installed inside the tank (2), and a working device that cooperates with the triggering device is installed above the triggering device. The triggering device includes an installation pipe (400) fixedly installed on the inner top wall of the tank (2), and a pressure plate (401) that can be reciprocated in a sealable manner is installed inside the installation pipe (400). A support spring (402) is fixedly installed between the pressure plate (401) and the inner top wall of the tank (2). The working device includes a through hole (500) installed on the inner top wall of the tank (2), and a linkage rod (501) that can be reciprocated in a sealable manner is installed inside the through hole (500). A fifth venting steel pipe (502) is connected to the first venting steel pipe (103), and the other end of the fifth venting steel pipe (502) is connected to an external nitrogen storage tank. The linkage rod (501) A connecting plate (503) is fixedly installed on the top of the device. A mating block (504) is fixedly installed on the connecting plate (503). A spiral groove (505) is provided in the mating block (504). A spiral rod (506) is provided in the spiral groove (505). A rotating shaft (507) is fixedly installed at the upper end of the spiral rod (506). A working hole (508) communicating with the inside of the fifth vent steel pipe (502) is provided on the side of the device. The rotating shaft (507) can rotate in the working hole (508). The outer peripheral wall of the rotating shaft (507) and the inner peripheral wall of the working hole (508) are always sealed. A working disc (510) for blocking the communication inside the fifth vent steel pipe (502) is fixedly installed on the side of the rotating shaft (507).

2. The method for producing Fmoc-O-tert-butyl-L-glutamic acid according to claim 1, characterized in that: The nitrogen filling device includes a first air pump (100) placed on one side of the tank (2), a second air pump (101) placed above the first air pump (100), a third connecting hole (102) connected to the inside of the tank (2) on the top surface of the tank (2), a first venting steel pipe (103) connected to the third connecting hole (102), the other end of the first venting steel pipe (103) connected to the outlet end of the first air pump (100), and a second venting steel pipe (104) connected to the inlet end of the first air pump (100). The second air pump (101) is connected to an external nitrogen storage tank. The inlet end of the second air pump (101) is connected to a third vent steel pipe (105), which is connected to the first vent steel pipe (103). The outlet end of the second air pump (101) is connected to a fourth vent steel pipe (106), which is connected to an external nitrogen storage tank. The first air pump (100) is used to fill the tank body (2) with nitrogen from the external nitrogen storage tank. The second air pump (101) is used to fill the tank body (2) with nitrogen back into the external nitrogen storage tank.

3. The method for producing Fmoc-O-tert-butyl-L-glutamic acid according to claim 1, characterized in that: A positioning plate (600) is fixedly installed on the side of the fifth ventilation steel pipe (502), and a positioning groove (601) is provided on the positioning plate (600). A slider (602) that can reciprocate within the positioning groove (601) is fixedly installed on the connecting plate (503).

4. The method for producing Fmoc-O-tert-butyl-L-glutamic acid according to claim 2, characterized in that: A reciprocating push plate (700) is provided inside the first ventilation steel pipe (103). A baffle plate (701) is fixedly provided on the bottom surface of the push plate (700). A first flow hole (702) is provided in the middle of the push plate (700). A second flow hole (703) and a sealing gasket (704) are provided on the baffle plate (701), and the second flow hole (703) is located above the sealing gasket (704).

5. The method for producing Fmoc-O-tert-butyl-L-glutamic acid according to claim 1, characterized in that: The outer peripheral wall of the working disc (510) is fixedly provided with a first sealing ring (610), and the inner peripheral wall of the fifth vent steel pipe (502) is fixedly provided with a second sealing ring (611) for cooperating with the first sealing ring (610).

6. The method for producing Fmoc-O-tert-butyl-L-glutamic acid according to claim 2, characterized in that: The first ventilation steel pipe (103) has a stroke groove (800) on each side of its inner wall. The push plate (700) has a stroke block (801) fixedly installed on each side of its inner wall. The stroke block (801) can reciprocate within the stroke groove (800). A return spring (802) is fixedly installed between the stroke block (801) and the inner wall of the stroke groove (800).

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