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Preparation of 3,3-dimethyl butyryl chloride

A technology of dimethyl butyryl chloride and dimethyl butyric acid, which is applied in the preparation of carboxylic acid anhydride and organic chemistry, can solve the problems of large amount of thionyl chloride, serious equipment corrosion, and large environmental impact, and achieve short reaction time , low production cost and low environmental impact

Inactive Publication Date: 2011-04-27
XIAMEN UNIV
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0003] The purpose of the present invention is to aim at the existing preparation 3, the method for 3-dimethylbutyryl chloride has a large amount of thionyl chloride, serious equipment corrosion, and a large amount of sulfur dioxide gas will be released during operation, which has a greater impact on the environment. , higher production costs, etc., provide a method for preparing 3,3-dimethylbutyryl chloride with simple process, easy operation, high safety, low production cost and little impact on the environment

Method used

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  • Preparation of 3,3-dimethyl butyryl chloride

Examples

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Embodiment 1

[0013] Embodiment 1: In a 500ml four-necked flask with an electric stirrer, a thermometer and a reflux condenser, add 3,3-dimethylbutanoic acid 46.4g (0.4mol), start stirring, dropwise at room temperature After the dropwise addition of 27.47g (0.2mol) of phosphorus trichloride was completed, the temperature was raised to 60°C for 2 hours. After the reaction was completed, it was cooled to room temperature, and placed in a separatory funnel to separate layers. Take the upper layer and collect the fraction at 79-81°C by vacuum distillation at an absolute pressure of 20KPa to obtain 46.91g of 3,3-dimethylbutyryl chloride product with a yield of 87.12%.

Embodiment 2

[0014] Embodiment 2: reaction device and operation method are the same as embodiment 1. The difference is that the amount of phosphorus trichloride added is 18.26g (0.133mol). As a result, 42.54 g of 3,3-dimethylbutyryl chloride was obtained, with a yield of 79.01%.

Embodiment 3

[0015] Embodiment 3: reaction apparatus and operation method are the same as embodiment 1. The difference is that the amount of phosphorus trichloride added is 36.67g (0.267mol). As a result, 48.94 g of 3,3-dimethylbutyryl chloride was obtained with a yield of 90.89%.

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Abstract

Disclosed is a method to prepare 3, 3-dimethyl butyric acid chloride, relating to an organically synthesized intermediated compound and particularly relating to a method to prepare 3, 3-dimethyl butyric acid chloride from 3,3-dimethyl butyric acid and phosphorus trichloride. The invention provides a method to prepare 3, 3-dimethyl butyric acid chloride, which is simple in process, simple in operation and low in cost, with high safety and little pollution to the environment. 3,3-dimethyl butyric acid is added into a reactor and phosphorus trichloride is added while stirring; then the mixture is heated to react; the mixture is cooled to room temperature after reaction and then is kept still for delamination; after delamination, orthophosphorous acid at the lower layer is regarded as byproduct, and acyl chloride crude product at the upper layer is distillated under absolute pressure 20KPa through reduced pressure distillation and the distillate at 79-81 DEG C is collected; in this way, 3, 3-dimethyl butyric acid chloride can be obtained.

Description

technical field [0001] The invention relates to an organic synthesis intermediate, in particular to a method for preparing 3,3-dimethylbutyryl chloride by reacting 3,3-dimethylbutyric acid and phosphorus trichloride. Background technique [0002] 3,3-Dimethylbutyryl chloride is an important intermediate in organic synthesis, which is mainly used in the fields of pesticide and pharmaceutical industry. 3,3-dimethylbutyryl chloride can be prepared by reacting 3,3-dimethylbutyric acid with thionyl chloride or phosgene (US2034850, CN1778789A, Journal of Organic Chemistry1982, 47(12):2413-19). However, the amount of thionyl chloride is large, the equipment is severely corroded, and a large amount of sulfur dioxide gas is released during operation, which has a greater impact on the environment and higher production costs. The use of phosgene is a highly toxic gas, which is inconvenient to transport and use, which seriously affects safe production and environmental protection. 3,3...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C53/42C07C51/56
Inventor 黎四芳陈国钦
Owner XIAMEN UNIV
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