A 4-formyl-n-isopropylbenzamide two-vessel cross reaction system

Abstract

The utility model relates to a kind of 4-formyl-N-isopropyl benzamide double-kettle cross reaction system, including receiving tank, receiving tank is connected condenser and reaction kettle one respectively, condenser and reaction kettle one constitute circulation loop, reaction kettle one outlet is connected centrifuge inlet and reaction kettle two inlets respectively, reaction kettle two outlet is also connected reaction kettle one inlet, centrifuge is also connected oven;Reaction kettle one is connected 1,2-dichloroethane storage tank, N, N-dimethylformamide storage tank, thionyl chloride storage tank, methyl tert-butyl ether storage tank, nitrogen main pipe respectively;Reaction kettle two is connected isopropylamine storage tank, hydrochloric acid storage tank, tap water main pipe, nitrogen main pipe respectively.The reaction system of the utility model preparation 4-formyl-N-isopropyl benzamide greatly shortens reaction time and raw material reaction is complete, greatly reduces production cost, reaction kettle one and reaction kettle two constitute double-kettle cross structure, greatly shorten washing stratification time, reduce Vocs volatilization, and production site environment is friendly.

Description

Technical Field

[0001] This utility model belongs to the field of fine chemical technology application technology, specifically relating to a 4-formyl-N-isopropylbenzamide dual-reactor cross-reaction system. Background Technology

[0002] 4-Formyl-N-isopropylbenzamide is an important pharmaceutical intermediate in the chemical industry. Currently, the general production process for 4-formyl-N-isopropylbenzamide is as follows: p-Aldehydebenzoic acid, thionyl chloride, and 1,2-dichloroethane are heated to 75-85°C and refluxed for 12 hours. The mixture is then cooled to room temperature, concentrated under reduced pressure to remove 1,2-dichloroethane and excess thionyl chloride, followed by the addition of dichloromethane. The mixture is then frozen to 0-5°C, and isopropylamine is added dropwise. The reaction is maintained at this temperature for 2 hours. The mixture is washed with saturated brine, the aqueous phase is discarded, and the organic phase is concentrated under reduced pressure to remove dichloromethane. Finally, ethyl acetate is added, and the mixture is recrystallized, centrifuged, and vacuum dried to obtain the final product. This production process has the following disadvantages: (1) The reaction time is long and the main raw material p-aldehyde benzoic acid does not react completely.

[0003] (2) Excess thionyl chloride volatilizes significantly during vacuum concentration, resulting in a harsh on-site environment.

[0004] (3) Distillation recovery of 1,2-dichloroethane contains thionyl chloride, and distillation recovery of dichloromethane contains isopropylamine, which is not conducive to production and application, and the production cost is high.

[0005] (4) Using saturated brine to wash the organic phase results in wastewater with high salt content, which is difficult to treat.

[0006] (5) The product yield is low, and a large amount of product dissolves in the waste liquid, making it difficult to recycle. Summary of the Invention

[0007] The purpose of this invention is to overcome the above-mentioned shortcomings and provide a 4-formyl-N-isopropylbenzamide dual-reactor cross-reaction system, which has the advantages of short reaction time, high raw material utilization rate, high product yield, low production cost, and environmentally friendly production site.

[0008] The technical solution adopted by this utility model to solve the above problems is as follows: a 4-formyl-N-isopropylbenzamide dual-reactor cross-reaction system, including a receiving tank, which is connected to a condenser and a first reaction vessel respectively. The condenser and the first reaction vessel form a circulation loop. The outlet of the first reaction vessel is connected to the inlet of a centrifuge and the inlet of a second reaction vessel respectively. The outlet of the second reaction vessel is also connected to the inlet of the first reaction vessel. The first reaction vessel and the second reaction vessel form a dual-reactor cross-reaction structure. The outlet of the centrifuge is connected to an oven and a ton container respectively. The ton container is also connected to the first reaction vessel via a diaphragm pump.

[0009] Preferably, the first reactor is also connected to a 1,2-dichloroethane storage tank, an N,N-dimethylformamide storage tank, a thionyl chloride storage tank, a methyl tert-butyl ether storage tank, and a nitrogen main pipe; the second reactor is also connected to an isopropylamine storage tank, a hydrochloric acid storage tank, a tap water main pipe, and a nitrogen main pipe.

[0010] Preferably, both the inlet and outlet pipes of reactor one and reactor two are equipped with regulating valves.

[0011] Preferably, both reactor one and reactor two are glass-lined reactors.

[0012] Preferably, both reactor one and reactor two are equipped with glass sight glasses below their bottom valves.

[0013] Preferably, the outlet pipe of the condenser is equipped with a reflux regulating valve and an outlet regulating valve.

[0014] Preferably, the centrifuge is a stainless steel centrifuge.

[0015] Preferably, the oven is a vacuum drying oven.

[0016] Compared with the prior art, the advantages of this utility model are: (1) The present invention provides a dual-reactor cross-reaction system for the preparation of 4-formyl-N-isopropylbenzamide, which greatly shortens the reaction time, ensures complete reaction of raw materials, significantly improves the utilization rate of raw materials, and greatly reduces the production cost.

[0017] (2) In the 4-formyl-N-isopropylbenzamide double-reactor cross reaction system of this utility model, the outlet of reactor one is connected to the inlet of reactor two, and the outlet of reactor two is connected to the inlet of reactor one. Reactor one and reactor two form a double-reactor cross structure. This setting shortens the washing and stratification operation time, reduces labor intensity, reduces VOCs volatilization, and provides good environmental protection at the production site. Attached Figure Description

[0018] Figure 1 This is a schematic diagram of the structure of the 4-formyl-N-isopropylbenzamide dual-reactor cross-reaction system in an embodiment of this utility model.

[0019] Wherein: 1 is the receiving tank, 2 is the condenser, 3 is the first reaction vessel, 4 is the centrifuge, 5 is the second reaction vessel, and 6 is the drying oven. Detailed Implementation

[0020] The present invention will be further described in detail below with reference to the accompanying drawings and embodiments.

[0021] like Figure 1 The diagram shown is a schematic representation of the 4-formyl-N-isopropylbenzamide dual-reactor cross-reaction system in this embodiment.

[0022] A 4-formyl-N-isopropylbenzamide dual-reactor cross-reaction system includes a receiving tank 1, which is connected to a condenser 2 and a reaction vessel 3. The condenser 2 and the reaction vessel 3 form a circulation loop. The outlet of the reaction vessel 3 is connected to the inlet of a centrifuge 4 and the inlet of a second reaction vessel 5. The outlet of the second reaction vessel 5 is also connected to the inlet of the first reaction vessel 3. The reaction vessel 3 and the second reaction vessel 5 form a dual-reactor cross-reaction structure. The outlet of the centrifuge 4 is connected to an oven 6 and a ton container. The ton container is also connected to the first reaction vessel 3 via a diaphragm pump.

[0023] The reactor 3 is also connected to a 1,2-dichloroethane storage tank, an N,N-dimethylformamide storage tank, a thionyl chloride storage tank, a methyl tert-butyl ether storage tank, and a nitrogen main pipe, respectively; the reactor 5 is also connected to an isopropylamine storage tank, a hydrochloric acid storage tank, a tap water main pipe, and a nitrogen main pipe, respectively.

[0024] Both the inlet and outlet pipes of reactor 3 and reactor 5 are equipped with regulating valves.

[0025] Both reactor 3 and reactor 5 are glass-lined reactors.

[0026] Both reactor 3 and reactor 5 are equipped with glass sight glasses below their bottom valves.

[0027] The outlet pipe of the condenser 2 is equipped with a reflux regulating valve and an outlet regulating valve.

[0028] The centrifuge 4 is a stainless steel centrifuge.

[0029] The oven 6 is a vacuum drying oven.

[0030] The working process of this embodiment will be described in detail below with reference to the accompanying drawings: 1. Add a certain amount of p-aldehyde benzoic acid (bagged solid), 1,2-dichloroethane (including fresh 1,2-dichloroethane and recovered 1,2-dichloroethane) from the 1,2-dichloroethane storage tank, thionyl chloride from the thionyl chloride storage tank, and N,N-dimethylformamide from the N,N-dimethylformamide storage tank into reactor 3, and start stirring in reactor 3.

[0031] 2. The temperature of reactor 3 is raised to 75~85℃ and kept at this temperature for 2 hours. A portion of the vapor in reactor 3 is condensed into liquid by condenser 2 and flows back to reactor 3.

[0032] 3. Freeze the reactor to 0~5℃.

[0033] 4. Add the isopropylamine from the isopropylamine storage tank into reactor 2, open the nitrogen valve on reactor 2, and let the nitrogen enter reactor 2 through the nitrogen main pipe. When the pressure inside the reactor reaches 0.05~0.1MPa, close the nitrogen valve.

[0034] 5. Maintain the temperature of reactor 3 at 0~5℃. Open the outlet valve of reactor 2 (5) and the inlet valve of reactor 3, and drip the isopropylamine transfer material from reactor 2 (5) into reactor 3. After dripping, maintain the temperature for 2 hours.

[0035] 6. Add tap water from the tap water pipe and hydrochloric acid from the hydrochloric acid storage tank into reactor 2, stir to dissolve, and obtain dilute hydrochloric acid. Open the nitrogen valve on reactor 2, and nitrogen enters reactor 2 through the nitrogen main pipe. When the pressure inside the reactor reaches 0.05~0.1MPa, close the nitrogen valve.

[0036] 7. Open the outlet valve of reactor 25 and the inlet valve of reactor 13. Transfer the prepared dilute hydrochloric acid from reactor 25 to reactor 13, stir for 1 hour, and let stand for 1 hour.

[0037] 8. Open the nitrogen valve on reactor 3. Nitrogen gas enters reactor 3 through the nitrogen main pipe. When the pressure inside the reactor reaches 0.05~0.1MPa, close the nitrogen valve. Open the outlet valve of reactor 3 and the inlet valve of reactor 25 to transfer the lower organic phase material in reactor 3 to reactor 25. The upper wastewater is discharged into the sewage treatment plant for treatment.

[0038] 9. Pour tap water from the tap into reactor 25, stir for 1 hour, and let stand for 1 hour.

[0039] 10. Open the nitrogen valve on reactor 25 to pressurize the reactor to 0.05~0.1MPa, then close the nitrogen valve. Open the outlet valve of reactor 25 and the inlet valve of reactor 13 to transfer the lower organic phase material from reactor 25 to reactor 13. Discharge the upper wastewater into the sewage treatment plant for treatment.

[0040] 11. The reaction vessel 3 is heated to 75~85℃ and distilled at atmospheric pressure to remove 1,2-dichloroethane solvent. The 1,2-dichloroethane vapor in the reaction vessel 3 is condensed into liquid by condenser 2 and collected to receiving tank 1 to obtain recovered 1,2-dichloroethane, which is then packed into barrels for use in the production of this product.

[0041] 12. Add the methyl tert-butyl ether (including fresh methyl tert-butyl ether and recycled methyl tert-butyl ether) from the methyl tert-butyl ether storage tank into reactor 3, heat to 50~60℃, stir until dissolved, and part of the vapor in reactor 3 is condensed into liquid by condenser 2 and flows back to reactor 3.

[0042] 13. Freeze the reactor to 0~5℃ and keep it at that temperature for 2 hours to allow crystals to precipitate.

[0043] 14. The liquid in the reactor 3 is transferred into the centrifuge 4 in several batches for centrifugation and filtration. The resulting filter cake is the wet product of 4-formyl-N-isopropylbenzamide.

[0044] 15. The filtrate after centrifugation is put into a ton container, and then returned to the reactor-3 through a diaphragm pump. The temperature is raised to 50~60℃ and the methyl tert-butyl ether solvent is distilled off under normal pressure. The methyl tert-butyl ether vapor in the reactor-3 is condensed into liquid by condenser 2 and collected to receiving tank 1 to obtain recovered methyl tert-butyl ether, which is then packed into barrels for use in the production of this product.

[0045] 16. Place the wet 4-formyl-N-isopropylbenzamide in oven 5 and vacuum dry it at 60~65℃ for 12 hours to obtain the finished 4-formyl-N-isopropylbenzamide product.

[0046] In addition to the above embodiments, this utility model also includes other implementation methods. All technical solutions formed by equivalent transformation or equivalent substitution should fall within the protection scope of the claims of this utility model.

Claims

1. A two-stage cross-reaction system for 4-formyl-N-isopropylbenzamide, characterized in that: It includes a receiving tank (1), which is connected to a condenser (2) and a reactor (3) respectively. The condenser (2) and the reactor (3) form a circulation loop. The outlet of the reactor (3) is connected to the inlet of a centrifuge (4) and the inlet of a reactor (5) respectively. The outlet of the reactor (5) is also connected to the inlet of the reactor (3). The centrifuge (4) is also connected to an oven (6). The first reactor (3) is also connected to a 1,2-dichloroethane storage tank, an N,N-dimethylformamide storage tank, a thionyl chloride storage tank, a methyl tert-butyl ether storage tank, and a nitrogen main pipe, respectively; the second reactor (5) is also connected to an isopropylamine storage tank, a hydrochloric acid storage tank, a tap water main pipe, and a nitrogen main pipe, respectively.

2. The 4-formyl-N-isopropylbenzamide dual-reactor cross-reaction system according to claim 1, characterized in that: Both the inlet and outlet pipes of reactor one (3) and reactor two (5) are equipped with regulating valves.

3. The 4-formyl-N-isopropylbenzamide dual-reactor cross-reaction system according to claim 1, characterized in that: Both reactor one (3) and reactor two (5) are glass-lined reactors.

4. The 4-formyl-N-isopropylbenzamide dual-reactor cross-reaction system according to claim 1, characterized in that: Both reactor one (3) and reactor two (5) are equipped with glass sight glasses under their bottom valves.

5. The 4-formyl-N-isopropylbenzamide dual-reactor cross-reaction system according to claim 1, characterized in that: The outlet pipe of the condenser (2) is equipped with a reflux regulating valve and an outlet regulating valve.

6. The 4-formyl-N-isopropylbenzamide dual-reactor cross-reaction system according to claim 1, characterized in that: The centrifuge (4) is a stainless steel centrifuge.

7. The 4-formyl-N-isopropylbenzamide dual-reactor cross-reaction system according to claim 1, characterized in that: The oven (6) is a vacuum drying oven.

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