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Synthesis process of methyl m-cyanomethyl benzoate

A technology of methyl cyanomethyl benzoate and synthesis process, which is applied in the field of synthesis process of methyl m-cyanomethyl benzoate, can solve the problems of non-environmental protection, high cost, and use of toxic reagents, and achieve less three wastes and low cost , high conversion efficiency

Pending Publication Date: 2022-07-29
JIANGSU RUIDA TECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to provide a kind of synthesis process of methyl m-cyanomethylbenzoate, which solves the problem that the method for preparing methyl m-cyanomethylbenzoate in the prior art is high in cost, not environmentally friendly, and uses toxic reagents The problem

Method used

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  • Synthesis process of methyl m-cyanomethyl benzoate
  • Synthesis process of methyl m-cyanomethyl benzoate

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Experimental program
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Embodiment 1

[0033] refer to figure 1 and figure 2 , a kind of synthesis technique of m-cyanomethyl methyl benzoate, comprises the following steps:

[0034] The first step, the chlorination reaction:

[0035] (1) Use CCl in a dry three-necked bottle 4 dissolving methyl m-toluate;

[0036] (2) Azobisisobutyronitrile and chlorosuccinimide were added to the reaction system in three times, and the time interval of each addition was 2-3h, and the temperature was raised to 70 °C for 8 hours; After the raw material point basically disappears, the reaction ends;

[0037] (3) filter to remove succinimide, and unreacted chlorosuccinimide, and the filtrate rotary evaporation obtains oil product A;

[0038] The second step, cyanation reaction:

[0039] (1) product A is added in the there-necked flask in the first step, sodium cyanide, potassium iodide and methyl alcohol are added, and stir;

[0040] (2) the temperature is raised to 60 DEG C and refluxed for 1 hour, and the reaction is monitore...

Embodiment 2

[0047] refer to figure 1 and figure 2 , a kind of synthesis technique of m-cyanomethyl methyl benzoate, comprises the following steps:

[0048] The first step, the chlorination reaction:

[0049] (1) Use CCl in a dry three-necked bottle 4 Methyl m-toluate is dissolved; the volume model of the three-necked flask is 100mL, wherein, the methyl m-toluate consumption is based on 19.86g, CCl 4 The dosage is based on 50mL;

[0050] (2) Azobisisobutyronitrile and chlorosuccinimide were added to the reaction system in three times, and the time interval of each addition was 2-3h, and the temperature was raised to 70 °C for 8 hours; After the raw material point basically disappeared, the reaction ended; the consumption of azobisisobutyronitrile was based on 0.58g, and the consumption of chlorosuccinimide was based on 17.66g;

[0051] (3) remove succinimide by filtration, and unreacted chlorosuccinimide, and the filtrate rotary evaporation obtains oily product A; the amount of oily ...

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Abstract

The invention relates to the technical field of pharmacy, in particular to a synthesis process of methyl m-cyanomethyl benzoate, and solves the problems that in the prior art, a method for preparing methyl m-cyanomethyl benzoate is high in cost and not environmentally friendly, and toxic reagents can be used. The invention relates to a synthesis process of methyl m-cyanomethyl benzoate. The synthesis process comprises the following steps: chlorination reaction and cyanidation reaction. According to the method, methyl m-methylbenzoate and chlorosuccinimide are taken as initial raw materials, the methyl m-cyanomethyl benzoate finished product is finally obtained through the working sections of chlorination, cyanidation and distillation, the product synthesis cost is low, the process steps are short, few three wastes are generated in the whole process, and compared with a traditional chlorine gas introduction process, the conversion efficiency is high, and the production cost is low. And the method is economical and environment-friendly, and has a good application prospect in the development of the pharmaceutical field.

Description

technical field [0001] The invention relates to the technical field of pharmacy, in particular to a synthesis process of methyl m-cyanomethylbenzoate. Background technique [0002] Methyl m-cyanomethyl benzoate is the key intermediate of synthesizing ketoprofen, and in the prior art, about the synthetic scheme of methyl m-cyanomethyl benzoate, there are following several: (1) with methyl m-bromobenzoate Ester and 4-isoxazole boronic acid are prepared by coupling reaction of raw materials, and the yield of this route reaches 69%, but the used 4-isoxazole boronic acid and the catalyst triphenylphosphine palladium chloride are relatively expensive; (2) with m-bromomethyl Methyl benzoate is raw material and NaCN or potassium cyanide are raw material preparation, this route is concise, and yield is high, but this route uses highly toxic substances sodium cyanide, potassium cyanide; (3) with m-bromomethylbenzene Methyl formate and trimethylsiliconitrile are prepared as raw materi...

Claims

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Application Information

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IPC IPC(8): C07C253/14C07C255/41
CPCC07C253/14C07C67/307C07C255/41C07C69/76
Inventor 周乔周苗冯亚兵马晨皓钟庆徐冬华江红涛朱良赵炯邱丽娟朱翔
Owner JIANGSU RUIDA TECH CO LTD