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Preparation method of medical intermediate 2,3,4-trimethoxy benzaldehyde

A technology of trimethoxybenzaldehyde and trihydroxybenzaldehyde, which is applied to pharmaceutical intermediates 2, to achieve the effects of increased market price, less equipment investment, and convenient industrial production

Active Publication Date: 2004-12-22
南京龙源天然多酚合成厂
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

2,3,4-Trimethoxybenzaldehyde The development and production of this product have not been reported in the literature so far

Method used

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  • Preparation method of medical intermediate 2,3,4-trimethoxy benzaldehyde

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Add 150 g of raw materials 2,3,4-trihydroxybenzaldehyde and an appropriate amount of water into a reactor with a thermometer, a stirrer and a heating jacket. After heating and dissolving, add the following materials into three times under stirring:

[0013] Concentration is 35% (weight) NaOH liquid 600mL, dimethyl sulfate 600g, catalyst trioctylmethylammonium chloride, tetrabutylammonium bromide 12g altogether.

[0014] The temperature in the reactor is maintained at 50-70°C, and the methylation reaction is carried out under stirring. After the methylation reaction was completed, the materials were allowed to stand and separate into layers. The upper layer was a yellow oil, and the lower layer was a mother liquor layer. After cooling, the mother liquor was removed, and the oil layer was washed with water to neutrality. The distillate was collected by distillation under reduced pressure, and 165 g of white crystals were obtained after cooling. . Through high-performance...

Embodiment 2

[0016] The preparation device is the same as in Example 1. Put 150g of 2,3,4-trihydroxybenzaldehyde into the reactor, dissolve at 50°C, add 25% NaOH aqueous solution 700mL, dimethyl sulfate 600g, phase transfer catalyst benzyltriethylammonium chloride and tetra 6g each of butylammonium bisulfate, after the methylation was completed, the crude product was separated, washed with water, and distilled to obtain the product.

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Abstract

A process for preparing the 2,3,4-trimethoxyphenyl formaldehyde as the intermediate of medicine includes the methylating reaction between 2,3,4-trihydroxyphenyl formaldehyde, dimethyl sulfate, quaternary ammonium salt and sodium hydroxide at 50-70 deg.C, laying aside for layering, taking the upper oily layer, water washing, vacuum distilling, cooling and crystallizing. Its advantages are high output rate and high purity.

Description

(technical field) [0001] The invention relates to a preparation method of compound 2,3,4-trimethoxybenzaldehyde as a pharmaceutical intermediate. (Background technique) [0002] 2,3,4-Trimethoxybenzaldehyde is a white crystalline powder with the chemical formula C 10 h 12 o 4 , with a molecular weight of 196.2 and a melting point of 38-40°C, is an important pharmaceutical intermediate, mainly used in new drugs Ca 2+ Synthesis of channel blockers. The drug can be selectively used in cerebral arteries to reduce the incidence of headaches, and has a certain demand in the European and American markets. 2,3,4-Trimethoxybenzaldehyde The development and production of this product have not been reported in literature so far. (Content of invention) [0003] The purpose of the present invention is to provide a method for preparing 2,3,4-trimethoxybenzaldehyde using gallic acid derivatives as raw materials, which can be applied to industrial production, provide high-purity produ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/71C07C47/575
Inventor 张宗和黄嘉玲徐浩李丙菊秦清仲崇茂
Owner 南京龙源天然多酚合成厂
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