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Preparing method for o-methoxybenzoyl chloride

A technology of o-methoxybenzoyl chloride and methoxybenzoyl chloride, applied in the field of preparation of o-methoxybenzoyl chloride, can solve the problems of inconvenient industrial production, unfavorable environmental protection, long reaction time, etc. The effect of mild operation, mild reaction, and mild reaction conditions

Inactive Publication Date: 2016-04-13
ZHEJIANG ESIGMA BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method has a long reaction time, the purity is difficult to improve (unreacted thionyl chloride is difficult to remove), the yield is also unsatisfactory, and it is not conducive to environmental protection, which brings inconvenience to industrialized production

Method used

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  • Preparing method for o-methoxybenzoyl chloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Add 15.23g (0.1mol) of o-methoxybenzoic acid, 30.5g of dichloroethane, and 0.3g (0.004mol) of DMF into a reaction vessel with a tail gas absorption device, raise the temperature to 40°C, and slowly add the concentration 2mol / L BTC-C 2 h 4 Cl 2 The solution was 15.5ml, and after the dropwise addition, the reaction was refluxed for 1 hour. After the solvent was recovered by distillation under reduced pressure, 16.88g of o-methoxybenzoyl chloride was obtained, with a content of 99.62% (gas chromatography), and a yield of 98.57%.

Embodiment 2

[0018] Add 15.23g (0.1mol) of o-methoxybenzoic acid, 45.7g of dichloroethane as a solvent, and 0.48g (0.006mol) of pyridine into a reaction vessel with a tail gas absorption device, raise the temperature to 42°C, and slowly add the concentration 2mol / L of BTC / C 2 h 4 Cl 2 The solution was 15.5ml, and after the dropwise addition, the reaction was refluxed for 1.5 hours. After the solvent was recovered by distillation under reduced pressure, 16.86g of o-methoxybenzoyl chloride was obtained, with a content of 99.68% (gas chromatography), and a yield of 98.28%.

Embodiment 3

[0020] Add 15.23g (0.1mol) of o-methoxybenzoic acid, 60.9g of dichloroethane, and 0.38g (0.005mol) of DMF into a reaction vessel with a tail gas absorption device, raise the temperature to 45°C, and slowly add the concentration 2mol / L of BTC / C 2 h 4 Cl 2 The solution was 15.5ml, and after the dropwise addition, the reaction was refluxed for 2 hours. After the solvent was recovered by distillation under reduced pressure, 16.92g of o-methoxybenzoyl chloride was obtained, with a content of 99.87% (gas chromatography), and a yield of 98.82%.

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Abstract

The invention provides a preparing method for o-methoxybenzoyl chloride and belongs to the technical field of carbon compounds. According to the method, o-methoxybenzoic acid serves as a raw material, triphosgene-C2H4C12 serves as a sulfonyl chlorination reagent, an initiator is added, and the mixture reacts at backflow temperature to prepare o-methoxybenzoyl chloride; the amount-of-substance concentration of a triphosgene-C2H4C12 solution is 2 mol / L, the feeding molar ratio of o-methoxybenzoic acid to the initiator to triphosgene is 1:(0.04-0.06):0.31, and the mass ratio of solvent dichloroethane to o-methoxybenzoic acid is (2-4):1. According to the preparing method, the reaction condition is mild, the technology is simple, operation is easy, the obtained product is high in purity and yield, and the method is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, in particular to a preparation method of o-methoxybenzoyl chloride. Background technique [0002] o-Methoxybenzoyl chloride (o-Methoxybenzoylchloride), also known as o-anisyl chloride, 2-methoxybenzoyl chloride, its structural formula is as follows: [0003] [0004] O-methoxybenzoyl chloride, appearance: white crystal, boiling point: 97-101°C, used in the synthesis of antihypertensive drug losartan. The present general known technique for producing o-methoxybenzoyl chloride is: reflux reaction with o-methoxybenzoic acid and sulfur oxychloride for 5-6 hours, rectification under reduced pressure to obtain o-methoxybenzoyl chloride, reaction A large amount of sulfur dioxide gas is produced in the process. The method takes a long time to react, the purity is difficult to improve (the unreacted thionyl chloride is difficult to remove), the yield is not ideal, and it is not conducive to...

Claims

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Application Information

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IPC IPC(8): C07C65/21C07C51/60
CPCC07C51/60C07C51/64C07C65/21
Inventor 吴中华张小朋陈贵才徐天华何奇雷闻鸣张丽佳
Owner ZHEJIANG ESIGMA BIOTECH CO LTD
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