Method for synthesizing (R)-2-chloropropionic acid by solid acid catalysis and trans-esterification reaction based on UIO-66

A UIO-66, solid acid catalyst technology, applied in chemical instruments and methods, carboxylate/lactone preparation, physical/chemical process catalysts, etc., can solve the problems of high industrial cost, low yield, environmental pollution, etc., To achieve the effect of being beneficial to environmental protection, less side reactions, and reducing production costs

Active Publication Date: 2017-05-31
HUBEI BIOCHEM PHARMA TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Purpose of the present invention will solve the problems such as the low yield of the preparation method of current (R)-2-chloropropionic acid, high industr

Method used

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  • Method for synthesizing (R)-2-chloropropionic acid by solid acid catalysis and trans-esterification reaction based on UIO-66

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] A method for the synthesis of (R)-2-chloropropionic acid based on UIO-66 solid acid catalyzed transesterification reaction of the present embodiment comprises the following steps:

[0024] (1) Solid acid catalyst SO 4 2- / Preparation of UIO-66

[0025] Weigh 0.053g ZrCl 4 and 0.034g of terephthalic acid were dissolved in 25mL of DMF (dimethylformamide), and then the above reactant was transferred to a polytetrafluoroethylene reactor, reacted at 120°C for 12h, filtered, and the precipitate was separated using DMF and Alternately washed with methanol, and dried the precipitate in an oven at 60°C for 12 hours to obtain UIO-66, then impregnated UIO-66 with 1.5mL sulfuric acid with a concentration of 1.5mol / L for 30min, filtered and dried, and placed in 500 The solid acid catalyst SO can be obtained in an oven at ℃ for 3 hours 4 2- / UIO-66;

[0026] (2) Preparation of (R)-2-chloropropionic acid

[0027] Add (R)-2-ethyl chloropropionate to the reactor, while stirring,...

Embodiment 2

[0030] A method for the synthesis of (R)-2-chloropropionic acid based on UIO-66 solid acid catalyzed transesterification reaction of the present embodiment comprises the following steps:

[0031] (1) Solid acid catalyst SO 4 2- / Preparation of UIO-66

[0032] Weigh 0.057gZrCl 4 and 0.034g of terephthalic acid were dissolved in 25mL of DMF (dimethylformamide), and then the above reactant was transferred to a polytetrafluoroethylene reactor, reacted at 110°C for 13h, filtered, and the precipitate was separated using DMF and Alternately washed with methanol, then dried the precipitate in an oven at 55°C for 13 hours to obtain UIO-66, then impregnated UIO-66 with 1.1mL of sulfuric acid with a concentration of 0.7mol / L for 30min, filtered and dried, and placed in 500 The solid acid catalyst SO can be obtained in an oven at ℃ for 3 hours 4 2- / UIO-66;

[0033] (2) Preparation of (R)-2-chloropropionic acid

[0034]Add (R)-2-ethyl chloropropionate to the reactor, while stirrin...

Embodiment 3

[0037] A method for the synthesis of (R)-2-chloropropionic acid based on UIO-66 solid acid catalyzed transesterification reaction of the present embodiment comprises the following steps:

[0038] (1) Solid acid catalyst SO 4 2- / Preparation of UIO-66

[0039] Weigh 0.055gZrCl 4 and 0.034g of terephthalic acid were dissolved in 25mL of DMF (dimethylformamide), and then the above reactant was transferred to a polytetrafluoroethylene reactor, reacted at 130°C for 11h, filtered, and the precipitate was separated using DMF and Alternately washed with methanol, and dried the precipitate in an oven at 65°C for 11 hours to obtain UIO-66, then impregnated UIO-66 with 2.2mL of sulfuric acid with a concentration of 1.5mol / L for 30min, filtered and dried, and placed in 500 The solid acid catalyst SO can be obtained in an oven at ℃ for 3 hours 4 2- / UIO-66;

[0040] (2) Preparation of (R)-2-chloropropionic acid

[0041] Add (R)-2-ethyl chloropropionate to the reactor, while stirrin...

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Abstract

The invention provides a method for synthesizing (R)-2-chloropropionic acid by a solid acid catalysis and trans-esterification reaction based on UIO-66. The method comprises the following steps: (1) preparation of a solid acid catalyst SO4<2>/UIO-66; and (2) preparation of (R)-2-chloropropionic acid. According to the method, UIO-66 is adopted as a solid acid catalyst of a substrate, the catalyst has strong acidity, so that the catalyst can effectively catalyze the trans-esterification reaction for synthesizing (R)-2-chloropropionic acid, the transformation rate is higher than 98%, side effects are less, and the catalyst can be used repeatedly, and therefore, the generation of tailings is effectively avoided, the production cost is lowered, and environmental protection is facilitated.

Description

technical field [0001] The invention relates to the technical field of preparation of (R)-2-chloropropionic acid, in particular to a method for synthesizing (R)-2-chloropropionic acid based on UIO-66 solid acid catalyzed transesterification reaction. Background technique [0002] 2-chloropropionic acid is one of the important intermediates in the synthesis of pesticides, dyes, medicines, nutritional supplements, etc. Its application involves many fields and is an important product. Because optical enantiomers are different in biological activity, toxicity, pharmacology, etc., the preparation of single enantiomers is extremely important. In recent years, with the rapid development of the chiral pharmaceutical market, the research and application of single enantiomer drugs It is also becoming more and more important, so the preparation of 2-chloropropionic acid with high optical purity is of great significance. [0003] At present, the preparation method of (R)-2-chloropropio...

Claims

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Application Information

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IPC IPC(8): C07C51/09C07C53/19B01J31/22
CPCB01J31/22C07C51/09C07C53/19
Inventor 周兴旺徐艳玲韩晓洵陈仁张闻艺
Owner HUBEI BIOCHEM PHARMA TECH
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