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Novel method for synthesizing 1-bromo-2,2-dimethoxypropane

A technology of dimethoxypropane and dichloromethane, which is applied in the field of biomedical intermediates, can solve the problems of difficult product purification, dangerous products, and low yield, and achieve easy purification, simple reaction operation, and improved reaction yield. Effect

Inactive Publication Date: 2020-06-30
TIANJIN QUANHECHENG TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The present invention proposes a new method for synthesizing 1-bromo-2,2-dimethoxypropane, which solves the problem of using dangerous goods, Problems of low yield and difficult product purification

Method used

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  • Novel method for synthesizing 1-bromo-2,2-dimethoxypropane
  • Novel method for synthesizing 1-bromo-2,2-dimethoxypropane
  • Novel method for synthesizing 1-bromo-2,2-dimethoxypropane

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Effect test

Embodiment 1

[0025] A new method for synthesizing 1-bromo-2,2-dimethoxypropane, comprising the following steps:

[0026] S1. Bromination reaction: Dissolve 12mL of acetone in 120mL of dichloromethane at room temperature, stir well, heat to 65°C, start to add 10g of bromine dropwise, and control the temperature at 65-75°C. After the dropwise addition, the reaction solution will Discoloration, stirred for 12 hours, and TLC detected that the reaction was complete. Add 1 times the volume of water to the reaction solution, separate the layers, extract 3 times with dichloromethane, wash the organic phase with sodium bicarbonate aqueous solution 2 times to weak alkalinity, then wash with saturated sodium chloride, and then wash with anhydrous sulfuric acid Sodium drying, spin-drying solvent, obtain product 1-bromoacetone 15.84g, yield 93%;

[0027] S2. Upprotection reaction: Dissolve 30g of 1-bromoacetone in 13mL of methanol at room temperature, add 26g of trimethyl orthoformate and 5.2g of conc...

Embodiment 2

[0029] A new method for synthesizing 1-bromo-2,2-dimethoxypropane, comprising the following steps:

[0030] S1. Bromination reaction: Dissolve 10mL of acetone in 120mL of dichloromethane at room temperature, stir evenly, heat to 65°C, start to add 10g of bromine dropwise, and control the temperature at 65-75°C. After the dropwise addition, the reaction solution will Discoloration, stirred for 11 h, and TLC detected that the reaction was complete. Add 1 times the volume of water to the reaction solution, separate the layers, extract 3 times with dichloromethane, wash the organic phase with sodium bicarbonate aqueous solution 2 times to weak alkalinity, then wash with saturated sodium chloride, and then wash with anhydrous sulfuric acid Sodium drying, spin-drying solvent, obtain product 1-bromoacetone 15.49g, yield 90.37%;

[0031] S2. Upprotection reaction: at room temperature, 26g of 1-bromoacetone was dissolved in 13mL of methanol, followed by adding 26g of trimethyl orthofo...

Embodiment 3

[0033] A new method for synthesizing 1-bromo-2,2-dimethoxypropane, comprising the following steps:

[0034] S1. Bromination reaction: Dissolve 14mL of acetone in 120mL of dichloromethane at room temperature, stir evenly, heat to 65°C, start to add 10g of bromine dropwise, and control the temperature at 65-75°C. After the dropwise addition, the reaction solution will Discoloration, stirred for 13h, and TLC detected that the reaction was complete. Add 1 times the volume of water to the reaction solution, separate the layers, extract 3 times with dichloromethane, wash the organic phase with sodium bicarbonate aqueous solution 2 times to weak alkalinity, then wash with saturated sodium chloride, and then wash with anhydrous sulfuric acid Sodium drying, spin-drying solvent, obtains product 1-bromoacetone 15.67g, yield 91.42%;

[0035] S2. Upprotection reaction: Dissolve 33.8g of 1-bromoacetone in 13mL of methanol at room temperature, add 26g of trimethyl orthoformate and 5.2g of c...

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Abstract

The invention belongs to the technical field of biomedical intermediates, and provides a novel method for synthesizing 1-bromo-2,2-dimethoxypropane, wherein the method comprises the following steps: S1, bromination reaction: dissolving acetone in dichloromethane, preheating to 65 DEG C, adding bromine, controlling the temperature at 65-75 DEG C, and carrying out a reaction for 11-13 h to obtain 1-bromoacetone; S2, carrying out an up-protection reaction: dissolving 1-bromoacetone in methanol, adding trimethyl orthoformate and concentrated hydrochloric acid, and carrying out a reaction for 2-3 hto obtain 1-bromo-2,2-dimethoxypropane. By means of the technical scheme, the problems that in the prior art, hazardous materials are used in a method for synthesizing 1-bromo-2,2-dimethoxypropane, the yield is low, and a product is difficult to purify are solved.

Description

technical field [0001] The invention belongs to the technical field of biomedical intermediates, and relates to a new method for synthesizing 1-bromo-2,2-dimethoxypropane. Background technique [0002] 1-Bromo-2,2-dimethoxypropane is an important biomedical intermediate, which can be widely used in the synthesis of various drugs. It has a small molecular weight and unique structure, and can be derived from a variety of downstream products. use. At present, the method for synthesizing 1-bromo-2,2-dimethoxypropane has the following defects: (1) involves the use of dangerous goods, such as phosphorus tribromide, concentrated sulfuric acid, etc.; (2) the reaction yield is low, Generally no more than 40%; (3) the product is difficult to purify; the manufacturers of 1-bromo-2,2-dimethoxypropane are very few, and the price is expensive, which seriously hinders the development of its downstream products and its application in the field of biomedicine further development. Content...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/56C07C43/313
CPCC07C41/56
Inventor 杜池敏
Owner TIANJIN QUANHECHENG TECH
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