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A kind of method for continuous synthesis of tetrahydrofuran-3-one

A technology of tetrahydrofuran and catalyst, which is applied in the field of continuous synthesis of tetrahydrofuran-3-one, can solve the problems of difficult operation, long reaction route, process pollution and the like, and achieves the effects of simple production process, easy industrial production and continuous production

Active Publication Date: 2022-08-02
上海巽田科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method needs to react with sulfuric acid solution and ceric sulfate as catalyst in the reaction kettle, which is a batch operation, and the sulfuric acid aqueous solution is corrosive after the reaction and causes great pollution.
[0004] In summary, the current methods for preparing tetrahydrofuran-3-one generally have long reaction routes, serious process pollution, and difficult operations.

Method used

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Examples

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Effect test

preparation example Construction

[0043] In the method for preparing tetrahydrofuran-3-one according to the present invention, 1,4-butynediol is used as a raw material to prepare tetrahydrofuran-3-one through dehydration, hydration and rearrangement. The product obtained in step 2) was passed through a 0.22 μm filter membrane and analyzed and detected by gas chromatography (GC). Gas chromatography detection conditions: Instrument: Shimadzu GC2010Plus, chromatographic column: Intercap-FFAP, 30m×0.25mm×0.25um, vaporization chamber temperature 250°C, FID temperature 300°C, column oven temperature program: 60°C for 1min, and then The temperature was raised to 230°C at a rate of 15°C / min for 10min. The product was qualitatively analyzed by gas chromatography-mass spectrometry (GC-MS) and the standard GC retention time control, and it was determined that the reaction product was mainly tetrahydrofuran-3-one. The product was quantitatively determined by Shimazu-GC 2010plus gas chromatography, and quantitative analys...

preparation Embodiment 1

[0050] ZSM-5 molecular sieve was first calcined at 500 °C for 5 h, then ion-exchanged at 85 °C for 3 times for 12 h in an aqueous ammonium nitrate solution (2 mol / L), and then calcined at 550 °C for 3 h to obtain H-ZSM-5. Weigh 0.275 g of chloroauric acid into a beaker, add 8.75 g of deionized water, and mix well. 5 g of HZSM-5 molecular sieves were weighed into the above solution, stirred for 24 h, filtered, and dried in an oven at 120°C overnight. The above catalyst powder was placed in a muffle furnace and heated to 200°C for 3 hours, and then heated to 300°C for 3 hours at a rate of 3°C / min. Au / ZSM-5 catalyst was prepared.

preparation Embodiment 2

[0052] ZSM-5 molecular sieve was first calcined at 500 °C for 5 h, then ion-exchanged at 85 °C for 3 times for 12 h in an aqueous ammonium nitrate solution (2 mol / L), and then calcined at 550 °C for 3 h to obtain H-ZSM-5. Weigh 0.33 g of chloroplatinic acid into a beaker, add 8.75 g of deionized water, and mix well. 5 g of HZSM-5 molecular sieves were weighed into the above solution, stirred for 24 h, filtered, and dried in an oven at 120°C overnight. The above catalyst powder was placed in a muffle furnace and heated to 200°C for 3 hours, and then heated to 300°C for 3 hours at a rate of 3°C / min. Pt / ZSM-5 catalyst was obtained.

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Abstract

The invention relates to a method for continuously synthesizing tetrahydrofuran-3-ketone. The method of the invention uses a specific catalyst, uses 1,4-butynediol as a raw material, and under mild conditions, realizes the coupling of hydration rearrangement and dehydration reaction, and directly prepares tetrahydrofuran-3-ketone. The catalyst provides two active sites: the metal active site catalyzes the hydration rearrangement of the alkyne bond, the acidic site catalyzes the dehydration and cyclization of the diol, and the synergistic effect between the two active sites realizes the one-step preparation of 1,4-butynediol Tetrahydrofuran-3-one. The method for continuously synthesizing tetrahydrofuran-3-ketone of the present invention has easy-to-obtain raw materials, greener route, simple process, high efficiency, and can be operated continuously.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a method for continuous synthesis of tetrahydrofuran-3-one. Background technique [0002] Tetrahydrofuran-3-one is an important pharmaceutical intermediate, which has a wide range of applications in the synthesis of cytotoxic drugs and antitumor drugs. In addition, it also has a wide range of uses in the spice and food industry. [0003] At present, the preparation methods of tetrahydrofuran-3-one mainly include the following: JP2006206463 (A) reported a method for obtaining tetrahydrofuran-3-one product through cyclization using 5-hydroxy-2,4-pentanedione as a reactant. The raw material 5-hydroxy-2,4-pentanedione is prepared by using aldehydes as raw materials, and it goes through three reaction steps in the middle, the route is long, the cost is high, and the poisonous potassium cyanide is used, which causes great pollution. CN101712664A reacts tert-butyl acetoacetate and br...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/32B01J23/50B01J23/68B01J23/72B01J29/44B01J29/46B01J31/08B01J37/02B01J37/03B01J37/08B01J37/30
CPCC07D307/32B01J29/44B01J29/46B01J23/682B01J23/50B01J31/08B01J23/72B01J37/30B01J37/0207B01J37/088B01J37/035B01J37/082
Inventor 牟新东刘晓然李慧
Owner 上海巽田科技股份有限公司
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