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Preparation process of veratone

A preparation process and veratrol technology are applied in the field of preparation technology of veratrol, which can solve the problems of low product yield and purity, and achieve the effects of stable quality, high yield and no environmental pollution.

Active Publication Date: 2014-07-23
SHANDONG HOLLY PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The shortcomings of the previous preparation process of veratrone: the previous process used D-dimethylmethyldopa as raw material, and under alkaline conditions, hypohalite was used as an oxidant to make D-dimethylmethyldopa Barba is converted into veratrone, but the yield and purity of the product are not very high, the highest is only 96%

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Example 1: Add 500 g of veratraldehyde and 435 g of methyl 2-chloropropionate into a 1000 ml beaker and stir at 25-35° C. to make the system clear and transparent to obtain liquid A for use.

[0014] Add 2000ml of toluene and 200g of solid sodium methoxide into a 5000ml washed and dried four-neck flask, stir, adjust the temperature to 30°C, add liquid A dropwise, control the temperature at 20-35°C, and complete the addition in about 3-5 hours After the addition, the temperature was raised to 40°C, and the temperature was kept at 35-50°C for 2 hours. After the heat preservation is over, control the temperature below 40°C, add 370ml of water, 565ml of liquid caustic soda, and 200ml of toluene, stir for 15 minutes, heat to evaporate the low-boiling solvent, and change to reflux when the gas phase temperature reaches 85°C, and keep at reflux for 1 hour.

[0015] After the heat preservation is over, cool down the system to 35°C, slowly add 870ml of hydrochloric acid dropwis...

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Abstract

The invention discloses a preparation process of veratrone, which uses veratraldehyde as the main raw material, first undergoes carboxylation of 2-chloropropionate methyl ester under the catalysis of sodium methoxide, then hydrolyzes under alkaline conditions, and decarboxylates with hydrochloric acid , and finally distilled to obtain the product. The product quality is stable and the yield is high. The molar yield of the product is 98%, and the main content is more than 98.5% through high-efficiency gas phase detection. The product does not change color when placed at room temperature for a long time. In addition, the toluene used in large quantities is easy to recycle, which is environmentally friendly and does not pollute the environment.

Description

technical field [0001] The invention specifically relates to a preparation process of veratrone. Background technique [0002] Veratrone, whose chemical name is 3,4-dimethoxypropiophenone, is a synthetic fragrance and an important pharmaceutical intermediate. It refers to the main raw material of nerve drugs and has a wide range of uses. At present, there are not many manufacturers at home and abroad, and the production methods are all extracted by veratraldehyde condensation hydrolysis. The method is similar, but the yield and purity of the product are very different, and the highest yield is 96%. Now compared with veratraldehyde and veratrone, the market price difference is not very big. If the yield and purity of veratrone are not high, there will be no profit, and the profit of veratraldehyde products can only be shifted backward. Therefore, many scientific research institutions and large-scale production enterprises are spending a lot of money to study detailed pr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C49/255C07C45/65
Inventor 李兰花裘月南沈林华王建荣蔺珍
Owner SHANDONG HOLLY PHARM CO LTD