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Process recovery method for veratrone

A technology of veratrone and process, which is applied in the field of industrial recovery of veratrone, a raw material of pharmaceutical intermediates, can solve the problems of increasing process safety risks and being unsuitable for large-scale production of enterprises, and achieves short reaction time, mild reaction conditions, and post-processing Handle simple effects

Pending Publication Date: 2022-07-01
SHANGHAI SYNCORES TECH INC +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the raw materials are relatively easy to obtain, potassium cyanide is used in the process, which is highly toxic and increases the safety risk of the process. At the same time, the by-products in this route release chloromethyl ether and dichloromethyl ether. These two strong carcinogens are not suitable for Enterprise scale production

Method used

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  • Process recovery method for veratrone
  • Process recovery method for veratrone
  • Process recovery method for veratrone

Examples

Experimental program
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Effect test

Embodiment 1

[0020] The solution containing 22g of Intermediate I was added to 50ml of ethanol, 6g of sodium hydroxide was added, the temperature was raised to 40-50°C, stirred for 16-18 hours, added with ethyl acetate, extracted, separated, washed, and concentrated to obtain 19.4g Veratrol, the yield is 99%.

Embodiment 2

[0022] The solution containing 22g of Intermediate I was added to 200ml, 6g of potassium hydroxide was added, the temperature was raised to 90-100°C, stirred for 12-14 hours, added with ethyl acetate, extracted, separated, washed, and concentrated to obtain 19.4g of quinoa Arutone, the yield is 99%.

Embodiment 3

[0024] The solid containing 22g of Intermediate I was added to 50ml of ethanol, 8g of potassium carbonate was added, 50ml of water was added, the temperature was raised to 60-70°C, stirred for 9-11 hours, filtered, added with ethyl acetate, extracted, separated, and washed , concentrated to obtain 18.6g veratrol, the yield was 95%.

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Abstract

The invention provides a method for recovering veratrone, which comprises the following steps: adding alkali or acid into solid or liquid containing an intermediate I or II, and hydrolyzing to obtain veratrone, the reaction formula is as follows:

Description

technical field [0001] The invention relates to the field of medicine and chemical industry, and relates to an industrial recovery method of veratrolone, a medicine intermediate raw material. Background technique [0002] Veratrol, also known as 3,4-dimethoxypropiophenone, has a wide demand in the additive market as a spice, and is also a common pharmaceutical intermediate raw material, such as an intermediate of antihypertensive drug methyldopa, Carbidopa intermediates, etc. Its structural formula is: [0003] According to literature reports, the production of veratrol is mainly as follows: [0004] (1) Using vanillaldehyde as the starting material, after methylation to obtain veratroaldehyde, it is condensed with nitroethane under n-butylamine, and then reduced with iron powder. The raw material price of this process route is too high, and the process will generate a large amount of waste slag iron powder, which is not suitable for green environmental protection requi...

Claims

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Application Information

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IPC IPC(8): C07C45/42C07C45/80C07C49/255
CPCC07C45/42C07C45/80C07C49/255
Inventor 廖文静黄鑫张志峰张继承黄鲁宁陈茜陶安平安建国顾虹
Owner SHANGHAI SYNCORES TECH INC
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