Synthetic method for drug intermediate m-chloroperbenzoic acid

A technology of m-chloroperoxybenzoic acid and chloroperoxybenzoic acid, which is applied in the preparation of pharmaceutical intermediates and the synthesis of m-chloroperoxybenzoic acid pharmaceutical intermediates, can solve the problem of endangering the health of production operators and increasing the risk of reaction process Factors, greater hazards to the health of operators, etc., to achieve the effects of safe production, shortened response time, and reduced equipment manufacturing costs

Inactive Publication Date: 2018-07-03
CHENGDU AO KA TE TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This synthetic method needs to adopt sodium hydroxide, hydrogen peroxide, sulfuric acid as reaction raw material, and sodium hydroxide has strong irritation and corrosiveness, and dust or smog can irritate eyes and respiratory tract, and direct contact of skin and eyes with NaOH can cause burns, therefore, use Sodium hydroxide as a reaction raw material will endanger the health of production operators and is not conducive to safe production
Hydrogen peroxide is an explosive and strong oxidant, which can react with combustibles to release a large amount of heat and oxygen, causing fire and explosion. Hydrogen peroxide is highly corrosive, and inhaling its vapor or mist is highly irritating to the respiratory tract, which will increase the risk factor of the reaction process and also Not conducive to safe production
Sulfuric acid is a highly corrosive solution, which requires high corrosion resistance for production equipment, which leads to an increase in equipment manufacturing costs, which is not conducive to reducing project costs; and the strong corrosive effect of sulfuric acid solution is very harmful to the health of operators

Method used

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  • Synthetic method for drug intermediate m-chloroperbenzoic acid
  • Synthetic method for drug intermediate m-chloroperbenzoic acid
  • Synthetic method for drug intermediate m-chloroperbenzoic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] The synthetic method of m-chloroperoxybenzoic acid medicine intermediate comprises the steps:

[0018] A: add 2mol m-chlorophenylacetamide in reaction vessel, 900ml mass fraction is 10% sodium nitrate solution, control stirring speed 230rpm, solution temperature is to 10 ℃, add 4mol mass fraction and be 15% methyl n-butyl ether solution, 4mol mass fraction is 20% 1,4-butanediol solution, add 4mol N-bromoacetamide in 2 times within 20min, and continue to react for 60min;

[0019] B: Then add 4mol aqueous solution, 2mol zinc fluoride powder, control stirring speed 310rpm, continue to react for 3h, add mass fraction and be 5% sodium chloride solution and wash 30min, mass fraction is 30% 3-heptanol solution and wash 20min, in mass fraction The fraction was recrystallized in 60% nitroethane solution and dehydrated with anhydrous sodium sulfate dehydrating agent to obtain 337.808 g of m-chloroperoxybenzoic acid with a yield of 98.2%.

Embodiment 2

[0021] The synthetic method of m-chloroperoxybenzoic acid medicine intermediate comprises the steps:

[0022] A: add 2mol m-chlorophenylacetamide in reaction vessel, 900ml mass fraction is 13% sodium nitrate solution, control stirring speed 240rpm, solution temperature is to 13 ℃, add 5mol mass fraction and be 19% methyl n-butyl ether solution, 5mol mass fraction is 23% 1,4-butanediol solution, add 5mol N-bromoacetamide in 3 times within 30min, and continue to react for 70min;

[0023] B: then add 5mol aqueous solution, 3mol zinc fluoride powder, control stirring speed 320rpm, continue reaction 3.5h, add mass fraction and be 8% sodium chloride solution and wash 40min, mass fraction is 4% 3-heptanol solution and wash 30min, in Recrystallize in 63% nitroethane solution and dehydrate with anhydrous sodium sulfate dehydrating agent to obtain 338.840 g of m-chloroperoxybenzoic acid with a yield of 98.5%.

Embodiment 3

[0025] The synthetic method of m-chloroperoxybenzoic acid medicine intermediate comprises the steps:

[0026] A: add 2mol m-chlorophenylacetamide in reaction vessel, 900ml mass fraction is 16% sodium nitrate solution, control stirring speed 260rpm, solution temperature is to 16 ℃, add 6mol mass fraction and be 22% methyl n-butyl ether solution, 6mol mass fraction is 26% 1,4-butanediol solution, add 6mol N-bromoacetamide in 4 times within 40min, and continue to react for 90min;

[0027] B: then add 6mol aqueous solution, 4mol zinc fluoride powder, control stirring speed 330rpm, continue to react for 4h, add mass fraction and be 11% sodium chloride solution and wash 50min, mass fraction is 37% 3-heptanol solution and wash 40min, in mass fraction The fraction was recrystallized in 65% nitroethane solution and dehydrated with anhydrous sodium sulfate dehydrating agent to obtain 339.528 g of finished m-chloroperoxybenzoic acid with a yield of 98.7%.

[0028] figure 1 It is the in...

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Abstract

The invention discloses a synthetic method for the drug intermediate m-chloroperbenzoic acid. The synthetic method comprises the following steps: adding m-chlorophenylacetamide and a sodium nitrate solution into a reaction vessel, controlling a stirring speed to be 230-260 rpm and a solution temperature to be 10-16 DEG C, adding a methyl n-butyl ether solution and a 1,4-butanediol solution, addingN-bromoacetamide in batches within 20-40 min, and continuing a reaction for 60-90 min; and then adding an aqueous solution and zinc fluoride powder, controlling a stirring speed to be 310-330 rpm, continue the reaction for 3-4 h, carrying out washing with a sodium chloride solution for 30-50 min, then carrying out washing with a 3-heptanol solution for 20-40 min, carrying out recrystallization ina nitroethane solution, and then carrying out dehydration with a dehydrating agent so as to obtain the finished m-chloroperoxybenzoic acid.

Description

technical field [0001] The invention relates to a preparation method of a pharmaceutical intermediate, which belongs to the field of organic synthesis, in particular to a synthesis method of a m-chloroperoxybenzoic acid pharmaceutical intermediate. Background technique [0002] M-chloroperoxybenzoic acid is mainly used as an oxidizing agent for synthetic pharmaceuticals, pesticides and other fine chemical products; it is used for cyclization reactions, Baeyer-Villiger reactions, N-oxidation reactions and S-oxidation reactions. Most of the existing synthetic methods are used in a reaction vessel, adding magnesium sulfate, sodium hydroxide, water, hydrogen peroxide, dioxane and ice cubes, the temperature is lowered to 15°C, stirring, adding m-chlorobenzoyl chloride, and then adding ice cubes , keep the temperature below 25°C, react for 15 minutes, add sulfuric acid, let stand, filter, distill off the solvent from the filtrate to obtain m-chloroperoxybenzoic acid. This synthet...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C407/00C07C409/30
CPCC07C407/00C07C409/30
Inventor 严义达
Owner CHENGDU AO KA TE TECH CO LTD
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