Method for preparing medical intermediate 4-hydroxy-3-methoxyphenylacetone

A technology for methoxyphenylacetone and intermediates, which is applied in the field of preparation of pharmaceutical intermediate 4-hydroxy-3-methoxyphenylacetone, can solve the problems of less research on synthetic methods, and achieve low price and low cost. Low, high-purity effect

Inactive Publication Date: 2018-05-04
SUZHOU GAIDE FINE MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

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Embodiment 1

[0022] A preparation method of pharmaceutical intermediate 4-hydroxyl-3-methoxyphenylacetone, comprising the following steps:

[0023] (1) preparation concentration is the zirconium acetate solution of 0.1moL / L, the chloroplatinic acid solution of 0.01moL / L; Concentration is the sodium hydroxide solution of 6g / L;

[0024] (2) disperse graphite oxide in deionized water, and ultrasonically disperse it for 30min under 1000W power, to obtain a graphene oxide dispersion;

[0025] (3) Mix and stir the zirconium acetate solution and the chloroplatinic acid solution prepared above, then add the graphene oxide dispersion, after stirring and mixing, add the sodium hydroxide solution dropwise, heat up to 30°C, stir and precipitate for 1h, and then The obtained mixed material was transferred to a hydrothermal kettle, and placed in a high-temperature oven at 120-°C for 8 hours of reaction. After the reaction, the reaction liquid in the hydrothermal kettle was filtered, and the obtained sol...

Embodiment 2

[0030] A preparation method of pharmaceutical intermediate 4-hydroxyl-3-methoxyphenylacetone, comprising the following steps:

[0031] (1) preparation concentration is the zirconium acetate solution of 0.4moL / L, the chloroplatinic acid solution of 0.05moL / L; Concentration is the sodium hydroxide solution of 11g / L;

[0032] (2) disperse graphite oxide in deionized water, and ultrasonically disperse it for 30min under 1000W power, to obtain a graphene oxide dispersion;

[0033] (3) Mix and stir the zirconium acetate solution and the chloroplatinic acid solution prepared above, then add the graphene oxide dispersion, after stirring and mixing, add the sodium hydroxide solution dropwise, heat up to 50°C, stir and precipitate for 2h, and then The obtained mixed material was transferred to a hydrothermal kettle, and placed in a high-temperature oven at 160°C for 8 hours of reaction. After the reaction, the reaction solution in the hydrothermal kettle was filtered, and the obtained s...

Embodiment 3

[0038] A preparation method of pharmaceutical intermediate 4-hydroxyl-3-methoxyphenylacetone, comprising the following steps:

[0039](1) preparation concentration is the zirconium acetate solution of 0.2moL / L, the chloroplatinic acid solution of 0.02moL / L; Concentration is the sodium hydroxide solution of 8g / L;

[0040] (2) disperse graphite oxide in deionized water, and ultrasonically disperse it for 30min under 1000W power, to obtain a graphene oxide dispersion;

[0041] (3) Mix and stir the above prepared zirconium acetate solution and chloroplatinic acid solution evenly, then add graphene oxide dispersion, after stirring and mixing, add sodium hydroxide solution dropwise, raise the temperature to 35°C, stir and precipitate for 1-2h, Then transfer the obtained mixed material to a hydrothermal kettle, and put it in a high-temperature oven at 130° C. for 7 hours of reaction. After the reaction, filter the reaction solution in the hydrothermal kettle, wash the obtained solid ...

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Abstract

The invention discloses a method for preparing a medical intermediate 4-hydroxy-3-methoxyphenylacetone. The method comprises steps as follows: firstly, a catalyst containing graphene, zirconia and Ptis prepared, 2-methoxy-4-(2-nitro-1-allyl) phenol is prepared from vanillic aldehyde and nitroethane as raw materials under the catalysis of glacial acetic acid and n-butylamine, and 2-methoxy-4-(2-oximido propyl) phenol is prepared from 2-methoxy-4-(2-nitro-1-allyl) phenol as a reaction raw material by adding ammonium formate and the self-made catalyst through stirring reaction; finally, 2-methoxy-4-(2-oximido propyl) phenol and a sulfuric acid solution are subjected to the stirring reaction for 1-3 h at the room temperature, after the reaction, a reaction liquid is left to stand for layering, a xylene layer is separated out and dried with anhydrous sodium sulfate, a solvent is removed through reduced-pressure concentration, fractions at 150-151 DEG C are collected, and 4-hydroxy-3-methoxyphenylacetone is obtained. The method is simple to operate, purity of a target product is high, yield is high, and cost is low.

Description

Technical field: [0001] The invention relates to the field of preparation of pharmaceutical intermediates, in particular to a preparation method of the pharmaceutical intermediate 4-hydroxyl-3-methoxyphenylacetone. Background technique: [0002] Phenyl and substituted phenylacetones are an important class of organic synthesis intermediates, widely used in the pharmaceutical industry, such as for the synthesis of sympathomimetic drugs, antianginal drugs, antihypertensive drugs and anticancer drugs. Among them, 4-hydroxy-3-methoxyphenylacetone is a key intermediate of carbidopa, a drug for treating Parkinson's syndrome. Compounds with biological activities such as treating osteoporosis and inhibiting cell mitosis can be synthesized by using it as a raw material. However, there are relatively few studies on its synthetic methods. Invention content: [0003] The purpose of this invention is to provide a kind of preparation method of pharmaceutical intermediate 4-hydroxyl-3-m...

Claims

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Application Information

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IPC IPC(8): C07C45/68C07C49/84B01J23/42
CPCB01J23/42C07C45/68C07C49/84
Inventor 李晓明
Owner SUZHOU GAIDE FINE MATERIALS CO LTD
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