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Fully continuous flow preparation method of 3-chloro-4-amyl oxoacetate

An amyl acetate, fully continuous technology is applied in the preparation of carboxylate, the preparation of organic compounds, the preparation of ester groups and hydroxyl groups, etc. The effect of shortened time, high degree of automation and improved reaction efficiency

Active Publication Date: 2021-06-18
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to overcome the deficiencies of long reaction time, large potential safety hazards, high energy consumption and low efficiency of the traditional batch synthesis method, the present invention provides a full continuous flow preparation method of 3-chloro-4-oxoamyl acetate, which The reaction time of the method is greatly shortened, the yield of the product 3-chloro-4-oxoamyl acetate is greatly increased, the automation degree and efficiency of the process are significantly improved, the energy consumption is greatly reduced, the safety is greatly improved, and industrialization is easy application

Method used

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  • Fully continuous flow preparation method of 3-chloro-4-amyl oxoacetate
  • Fully continuous flow preparation method of 3-chloro-4-amyl oxoacetate
  • Fully continuous flow preparation method of 3-chloro-4-amyl oxoacetate

Examples

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Embodiment 1

[0059]The acetylbutyrolactone liquid and the chlorine gas were simultaneously delivered to the Protrix microchannel reactor (the reaction volume was 4.2 ml, and the diameter of the microchannel was 2 mm), and the flow ratio of the acetylbutyrolactone liquid and the chlorine gas was adjusted so that the substrate acetylbutyrolactone The molar ratio of lactone (3) to chlorine is 1:1.3, the flow rate of acetylbutyrolactone liquid is 1.0 ml / min, the back pressure value of the back pressure valve is set to 0.2 Mpa, and the temperature in the Protrix microchannel reactor is controlled 25 ℃, after 30 seconds of reaction (that is, the residence time of the mixed reaction material in the microchannel reactor is 30 seconds), the mixed reaction material flows out from the outlet of the microchannel reactor, and after the gas component is separated by the gas-liquid separator, Collected in the product buffer tank. The conversion rate of sampling detection acetylbutyrolactone is 100%. The...

Embodiment 2

[0061] This embodiment is the same as Example 1, except that the only difference is that the micro-mixer before the acylation reaction in this embodiment is a T-type micro-mixer. In this example, the substrate acetylbutyrolactone was also completely converted, and the yield of the obtained product 3-chloro-4-oxoacetate amyl ester (1) was 89%, and the purity was 93% (GC).

Embodiment 3

[0063] This embodiment is the same as Example 1, except that the microchannel reactor used for the chlorination reaction in this embodiment is a tubular microchannel reactor with a volume of 5 milliliters and an internal diameter of 0.8 millimeters. In this example, the substrate acetylbutyrolactone was completely converted, and the yield of the obtained product 3-chloro-4-oxoacetate amyl ester (1) was 90.1%, and the purity was 96% (GC).

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Abstract

The invention belongs to the technical field of organic chemical engineering, and particularly relates to a fully continuous flow preparation method of 3-chloro-4-amyl oxoacetate. The method comprises the following steps of simultaneously conveying chlorine and a reaction solution of acetyl butyrolactone into a micro-channel reactor, and carrying out continuous chlorination reaction to obtain alpha-acetyl-alpha-chloro-gamma-butyrolactone, then continuously conveying the reaction liquid and a mixed solution of glacial acetic acid, hydrochloric acid and water to a micro-reaction system consisting of a next micro-mixer and a micro-channel reactor at the same time, and carrying out continuous acylation reaction to obtain 3-chloro-4-amyl oxoacetate finally, acquiring a final product in a micro-channel system of continuous quenching and continuous extraction separation. Compared with a traditional intermittent kettle type synthesis method, the method disclosed by the invention is short in reaction time, high in product yield, high in automation degree, high in process continuous efficiency, high in space-time yield, low in energy consumption and easy to industrially amplify and apply.

Description

technical field [0001] The invention belongs to the technical field of organic chemical engineering, and in particular relates to a preparation method of 3-chloro-4-oxoamyl acetate. Background technique [0002] Amyl 3-chloro-4-oxoacetate is an important fine chemical intermediate, which can be used to synthesize vitamin B 1 , has broad application prospects in industries such as medicine, pesticides and dyes. The structural formula of 3-chloro-4-oxoamyl acetate is as shown in (1) formula: [0003] [0004] Karaulova et al. ( Khimya Geterotsiklicheskikh Soedinenii, 1967, 1, 51) reported the synthesis of pentyl 3-chloro-4-oxoacetate (1) from α-acetyl-α-chloro-γ-butyrolactone and acetic anhydride in aqueous acetic acid and hydrochloric acid method, but the yield of compound (1) is only 71%. Hawksley et al. ( Journal of the Chemical Society, Perkin Transactions , 2001, 2, 144), Plazzi, P.V. et al. ( Farmaco, Edizione Scientifica, 1981, 11, 921), Vitali, T. et al....

Claims

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Application Information

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IPC IPC(8): C07C67/03C07C69/14B01J19/00
CPCC07C67/03C07D307/33B01J19/0093C07C69/14B01J2219/00867B01J2219/00894C07C67/10C07C69/63C07C67/31
Inventor 陈芬儿姜梅芬刘敏杰程荡俞超黄华山
Owner FUDAN UNIV
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