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A kind of full continuous flow preparation method of 3-chloro-4-oxoamyl acetate

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

Active Publication Date: 2022-03-18
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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  • A kind of full continuous flow preparation method of 3-chloro-4-oxoamyl acetate
  • A kind of full continuous flow preparation method of 3-chloro-4-oxoamyl acetate
  • A kind of full continuous flow preparation method of 3-chloro-4-oxoamyl acetate

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 specifically relates to a full continuous flow preparation method of 3-chloro-4-oxoamyl acetate. In the present invention, the reaction solution of chlorine gas and acetyl butyrolactone is simultaneously transported into the microchannel reactor, and continuous chlorination reaction is carried out to obtain α-acetyl-α-chloro-γ-butyrolactone; then the reaction solution continues to be mixed with ice The mixed solution of acetic acid, hydrochloric acid and water is delivered to the micro-reaction system formed by the next micro-mixer and micro-channel reactor at the same time, and the continuous acylation reaction is carried out to obtain 3-chloro-4-oxoamyl acetate; Quenching and continuous extraction are separated in a microchannel system to obtain the final product. Compared with the traditional batch synthesis method, the method of the invention has the advantages of short reaction time, high product yield, high degree of automation, high process continuous efficiency, high space-time yield, low energy consumption and easy industrial scale-up application.

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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Patent Type & Authority Patents(China)
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