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Method for preparing D-(+)-2-chloropropionyl chloride by adopting microchannel continuous flow reactor

A chloropropionyl chloride, microreactor technology, applied in chemical instruments and methods, chemical/physical/physical-chemical reactors, carboxylate preparation, etc., can solve the problem of large water content of L-lactic acid, low optical purity of products, synthesis Problems such as long steps, to achieve the effects of less by-products, high product purity, and less three wastes

Pending Publication Date: 2021-11-05
苏州永诺泓泽生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This route has high energy consumption, long synthesis steps, long time consumption and high cost
(2) Chinese patent document CN101284772A discloses a synthesis method using calcium fluoride as a basic catalyst, which reduces environmental pollution to a certain extent, but still has the disadvantages of low overall yield and low optical purity of the product
Due to the large water content of food-grade L-lactic acid, the method exothermic violently when amplified and mixed, has a high safety risk, and is not suitable for industrialized large-scale production; in addition, the method has a low yield, produces a large amount of waste water and waste residue, and the optical purity of the obtained product is low. , can not meet the requirements of preparing high-end medicine and material intermediates

Method used

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  • Method for preparing D-(+)-2-chloropropionyl chloride by adopting microchannel continuous flow reactor
  • Method for preparing D-(+)-2-chloropropionyl chloride by adopting microchannel continuous flow reactor

Examples

Experimental program
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Effect test

Embodiment 1

[0039] according to figure 1 Build a microchannel continuous flow reactor for reaction:

[0040] (1) Weigh 120g of L-lactic acid and add dichloromethane to a volume of 1L, add 12g of 2,6-di-tert-butylpyridine, and stir to obtain solution A;

[0041] (2) Weigh 300 g of thionyl chloride and add dichloromethane to a volume of 1 L, and stir to obtain solution B;

[0042] (3) The homogeneous solution A and the homogeneous solution B were respectively pumped into the micro-mixer at a flow rate of 0.5 mL / min, the mixing temperature was 5° C., and the reaction residence time was 40 minutes. After mixing, pass into the microreactor, the reaction temperature is controlled at 50°C, and the reaction residence time is 3 hours. Collect the effluent of the microreactor and obtain the D-(+)-2-chloropropionyl chloride fraction 161.9g after vacuum distillation to recover the solvent after normal pressure distillation; the yield is 96.4%; the product purity is 99.7%, and the optical purity rea...

Embodiment 2

[0044] according to figure 1 Build a microchannel continuous flow reactor for reaction:

[0045](1) Weigh 120g of L-lactic acid and add dichloromethane to a volume of 500mL, add 12g of 2,6-di-tert-butylpyridine, and stir to obtain solution A;

[0046] (2) Weigh 300g of thionyl chloride and add dichloromethane to a volume of 500mL, and stir to obtain solution B;

[0047] (3) The homogeneous solution A and the homogeneous solution B were respectively pumped into the micro-mixer at a flow rate of 0.5 mL / min, the mixing temperature was 5° C., and the reaction residence time was 40 minutes. After mixing, pass into the microreactor, the reaction temperature is controlled at 50°C, and the reaction residence time is 3 hours. Collect the effluent of the microreactor and obtain the D-(+)-2-chloropropionyl chloride fraction 159.5g after vacuum distillation to recover the solvent after normal pressure distillation; the yield is 95%; the product purity is 99.1%, and the optical purity re...

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Abstract

The invention is applicable to the technical field of organic intermediate preparation processes, and provides a method for preparing D-(+)-2-chloropropionyl chloride by adopting a microchannel continuous flow reactor, wherein the method comprises the steps: dissolving L-lactic acid and a catalyst 2,6-di-tert-butylpyridine in dichloromethane to obtain a homogeneous solution A; dissolving thionyl chloride in dichloromethane to obtain a homogeneous solution B; respectively and simultaneously pumping the homogeneous solution A and the homogeneous solution B into a micro-mixer in a micro-channel continuous flow reaction device; introducing a mixed solution of the micro-mixer in the micro-channel continuous flow reaction device into a micro-reactor; and collecting the effluent of the micro-reactor, recycling a solvent by normal pressure distillation, and carrying out reduced pressure distillation to obtain the D-(+)-2-chloropropionyl chloride with optical purity. The micro-channel continuous flow reactor used in the method is in full-automatic formation production, the control precision is high, the reaction process is safe and controllable, and the obtained D-(+)-2-chloropropionyl chloride is high in yield and high in optical purity; and the mass and heat transfer performance is good, the D-(+)-2-chloropropionyl chloride can be continuously prepared on a large scale, and the application prospect is wide.

Description

technical field [0001] The invention belongs to the technical field of organic intermediate preparation technology, and in particular relates to a method for preparing D-(+)-2-chloropropionyl chloride using a microchannel continuous flow reactor. Background technique [0002] D-(+)-2-chloropropionyl chloride is an important chemical raw material, which is widely used in the fields of medicine, pesticide and new materials. It can be used as the starting material for the synthesis of the anti-inflammatory and analgesic drug Cloxoprofen Sodium, the treatment of atopic dermatitis (eczema) Digotinib, the antihypertensive drug Perindopril, the hepatitis C drug Grazoprevir and various small peptides. D-(+)-2-chloropropionyl chloride is also an important intermediate for the preparation of parenteral nutrition agent alanyl glutamine. [0003] At present, the industrial production of D-(+)-2-chloropropionyl chloride still adopts the traditional kettle-type mechanically stirred batch...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/60C07C53/50B01J19/00
CPCC07C51/60C07B2200/07B01J19/0093C07C53/50
Inventor 阳应华季兵
Owner 苏州永诺泓泽生物科技有限公司
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