Synthetic method of 3,3-dimethyl butyladehyde

A technology of dimethyl butyraldehyde and a synthesis method, which are applied in 3 fields of preparation, can solve the problems of large consumption of thionyl chloride, serious equipment corrosion, and large environmental impact, and achieve short reaction time, low production cost, and small environmental impact. Effect

Inactive Publication Date: 2009-03-25
XIAMEN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The purpose of the present invention is to aim at the large amount of thionyl chloride existing in the method for preparing 3,3-dimethylbutyraldehyde, serious equipment corrosion, and a large amount of sulfur dioxide gas will be released during operati

Method used

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  • Synthetic method of 3,3-dimethyl butyladehyde
  • Synthetic method of 3,3-dimethyl butyladehyde

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Embodiment 1

[0014] 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 under the absolute pressure of 20KPa to obtain 46.91g of 3,3-dimethylbutyraldehyde product with a yield of 87.12%.

Embodiment 2

[0015] 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-dimethylbutyraldehyde was obtained with a yield of 79.01%.

Embodiment 3

[0016] 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-dimethylbutanal was obtained with a yield of 90.89%.

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Abstract

The invention provides a synthesizing method of 3, 3-dimethyl butyraldehyde, relates to an organic synthesis intermediate, particularly a method for preparing 3, 3-dimethyl butyraldehyde by the reaction of 3, 3-dimethylbutyric acid and phosphorus trichloride. A synthesizing method of 3, 3-dimethyl butyraldehyde with simple process, simple and convenient operation, high safety, low production cost and small influence to environment is provided. The method comprises the steps: the 3, 3-dimethylbutyric acid is added in a reactor and stirred, the phosphorus trichloride is added, then reaction is carried out after the temperature is raised to reaction temperature, after reaction, the reaction system is cooled to room temperature and stands for layering; and the lower layer of orthophosphorous acid divided after standing is taken as byproduct, the crude product of acyl chloride is adopted to carry out vacuum distillation under the absolute pressure of 20KPa and the distillate at 79 to 81 DEG C is collected, therefore the 3, 3-dimethyl butyraldehyde product is obtained.

Description

technical field [0001] The invention relates to an organic synthesis intermediate, in particular to a method for preparing 3,3-dimethylbutanal by reacting 3,3-dimethylbutyric acid and phosphorus trichloride. Background technique [0002] 3,3-Dimethylbutyraldehyde is an important intermediate in organic synthesis, which is mainly used in the fields of pesticides and pharmaceutical industries. 3,3-dimethylbutanal can be prepared by 3,3-dimethylbutyric acid and sulfur oxychloride or phosgene reaction (referring to U.S. Patent US2034850; Chinese patent CN1778789A; Journal of Organic Chemistry, 1982,47 (12 ): 2413-2419). 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 ...

Claims

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Application Information

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IPC IPC(8): C07C53/42C07C51/60
Inventor 黎四芳
Owner XIAMEN UNIV
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