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Synthetic method of n-heptyl chloroformate

A synthetic method, the technology of n-heptyl ester, applied in the field of chemistry, can solve the problem of many by-products, etc., and achieve the effect of simple process, reduced generation and high yield

Pending Publication Date: 2021-02-19
湖南维摩新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are many by-products produced during the synthesis of n-heptyl chloroformate at present, so it needs to be improved

Method used

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Experimental program
Comparison scheme
Effect test

Embodiment Construction

[0016] In order to make the above objects, features and advantages of the present invention more obvious and understandable, the following will clearly and completely describe the technical solutions in the embodiments of the present invention.

[0017] A kind of synthetic method of n-heptyl chloroformate:

[0018] 1. Experimental equipment and reagents

[0019] 1000ml four-port glass reaction flask, PTFE stirring and stirring governor, ±50°C thermometer, low temperature and constant temperature reaction bath, LZB glass rotameter, tail gas absorption bottle; n-octanol, 10% liquid caustic soda.

[0020] 2. Synthesis method

[0021] Reaction formula

[0022] CH 3 CH 2 CH 2 CH 2 CH 2 CH 2 CH 2 OH+COCl 2 →CH 3 CH 2 CH 2 CH 2 CH 2 CH 2 CH 2 OCOCl+HCl

[0023] 1. Throw 448g of n-heptanol into a 1000ml four-necked reaction flask at the bottom, adjust the low temperature and constant temperature reaction bath under stirring, and lower the temperature of the material ...

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Abstract

The invention discloses a synthetic method of n-heptyl chloroformate. The synthetic method comprises the steps of 1, adding 448 parts by weight of n-heptanol into a reaction container; 2, cooling n-heptanol to the temperature of -15+ / -1 DEG C, and then gradually introducing 505 parts by weight of phosgene, wherein when the accumulated introduction amount of phosgene is 0-300 parts by weight, the temperature in the reaction container is controlled to be less than or equal to -10 DEG C, when the accumulated introduction amount of phosgene is 300-430 parts by weight, the temperature in the reaction container is controlled to be greater than or equal to -10 DEG C and less than or equal to -5 DEG C, and when the cumulative introduction amount of phosgene is 430-505 parts by weight, the temperature in the reaction container is less than or equal to 2 DEG C; 3, when the accumulated flow of phosgene reaches 505 parts by weight, stopping introducing light, heating the material in the reaction container to the temperature of 20-25 DEG C, and keeping the temperature for 2 hours; 4, after heat preservation is completed, introducing nitrogen to remove excessive phosgene and hydrogen chloride, and obtaining a qualified n-heptyl chloroformate product. The method has the advantages of simple process, effective reduction of the generation of diester carbonate, safe and reliable production and high yield.

Description

technical field [0001] The invention relates to the field of chemistry, in particular to a method for synthesizing n-heptyl chloroformate. Background technique [0002] N-heptyl chloroformate is a chemical substance, which is mainly used as a chemical solvent, an amino protection agent, and the production of pharmaceuticals, herbicides and other chemical products. However, there are many by-products produced during the synthesis of n-heptyl chloroformate at present, so it needs to be improved. Contents of the invention [0003] The object of the present invention is to provide a kind of synthetic method of n-heptyl chloroformate, and the present invention process is simple, can effectively reduce the generation of carbonic diester, and production is safe and reliable and yield is higher. [0004] For solving the problems referred to above, technical scheme of the present invention is: [0005] A kind of synthetic method of n-heptyl chloroformate, comprises the steps: ...

Claims

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Application Information

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IPC IPC(8): C07C68/02C07C69/96
CPCC07C68/02C07C69/96
Inventor 胡晓珊杨云瑶张敦河刘亚龙
Owner 湖南维摩新材料有限公司