Preparation method for 4-trifluoromethylbenzyl chloride

A technology of p-trifluoromethylbenzyl chloride and p-chlorobenzotrifluoride, which is applied in the field of compound preparation, can solve the problems of low efficiency and high cost, and achieve the effects of reducing cost, short reaction process, and improving yield and production efficiency

Inactive Publication Date: 2018-03-13
江苏万隆科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, although there are multiple industrial methods for synthesizing p-trifluoromethyl benzyl chloride, most of them have the defects of higher cost or lower efficiency. How to provi

Method used

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  • Preparation method for 4-trifluoromethylbenzyl chloride
  • Preparation method for 4-trifluoromethylbenzyl chloride

Examples

Experimental program
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Embodiment 1

[0016] The concrete steps of the preparation method of trifluoromethylbenzyl chloride of the present embodiment comprise:

[0017] A. Add 150kg of pretreated tetrahydrofuran, 7.3kg of dried magnesium particles, 30g of iodine, 1kg of bromoethane and 0.5kg of p-chlorobenzotrifluoride into the reaction kettle, slowly feed nitrogen, stir and heat up to reflux, and keep reflux After 30 minutes, the Grignard reagent was successfully initiated, then the temperature was controlled at 50°C, and 44.5kg of p-chlorobenzotrifluoride was added dropwise. The reaction was controlled at 30°C for 6 hours, and then tetrahydrofuran was recovered, and the residue was cooled to room temperature and placed in 300 kg of ice water (18.5 kg of 35% hydrochloric acid aqueous solution was added to the ice water in advance). After fully hydrolyzed, the layers are separated, and the separated water layer is extracted once with 50L of toluene, and the organic matter obtained is combined with the separated or...

Embodiment 2

[0022] The concrete steps of the preparation method of trifluoromethylbenzyl chloride of the present embodiment comprise:

[0023] A. Add 150kg of pretreated tetrahydrofuran, 7.3kg of dried magnesium particles, 30g of iodine, 1kg of bromoethane and 0.5kg of p-chlorobenzotrifluoride into the reaction kettle, slowly feed nitrogen, stir and heat up to reflux, and keep reflux After 40 minutes, the Grignard reagent was successfully initiated, and then the temperature was controlled at 40°C, and 44.5kg of p-chlorobenzotrifluoride was added dropwise. The temperature was controlled at 20°C for 7 hours, then tetrahydrofuran was recovered, and the residue was cooled to room temperature and placed in 300 kg of ice water (18.5 kg of 35% hydrochloric acid aqueous solution was added to the ice water in advance). After fully hydrolyzed, the layers are separated, and the separated water layer is extracted once with 50L of toluene, and the organic matter obtained is combined with the separated...

Embodiment 3

[0026] The concrete steps of the preparation method of trifluoromethylbenzyl chloride of the present embodiment comprise:

[0027] A. Add 150kg of pretreated tetrahydrofuran, 7.3kg of dried magnesium particles, 30g of iodine, 1kg of bromoethane and 0.5kg of p-chlorobenzotrifluoride into the reaction kettle, slowly feed nitrogen, stir and heat up to reflux, and keep reflux After 20 minutes, the Grignard reagent was successfully initiated, then the temperature was controlled at 60°C, and 44.5kg of p-chlorobenzotrifluoride was added dropwise. The temperature was controlled at 40°C for 5 hours, then tetrahydrofuran was recovered, and the residue was cooled to room temperature and placed in 300 kg of ice water (18.5 kg of 35% hydrochloric acid aqueous solution was added to the ice water in advance). After fully hydrolyzed, the layers are separated, and the separated water layer is extracted once with 50L of toluene, and the organic matter obtained is combined with the separated org...

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Abstract

The invention relates to a preparation method for 4-trifluoromethylbenzyl chloride, wherein the preparation method comprises the specific steps: A, adding a proper amount of tetrahydrofuran, magnesium, iodine, bromoethane and p-chlorobenzotrifluoride into a reaction kettle, introducing nitrogen, stirring to rise the temperature to reflux, refluxing for 20 min-40 min, then controlling the temperature at 40 DEG C-60 DEG C, dropping p-trifluoromethyl chlorobenzene, after the dropping is finished, carrying out a heat preservation reaction for 1.5 h-3 h, then cooling to 5 DEG C-15 DEG C, adding a proper amount of paraformaldehyde, then controlling the temperature at 0 DEG C-60 DEG C, carrying out a reaction for 5 h-7 h, then recycling tetrahydrofuran, and carrying out reduced pressure distillation to obtain 4-trifluoromethylbenzyl alcohol; and B, adding a proper amount of hydrochloric acid and 4-trifluoromethylbenzyl alcohol into another reaction kettle, stirring to rise the temperature toreflux, carrying out a heat preservation reaction for 20 h-30 h, cooling to room temperature, stratifying, dehydrating, and carrying out reduced pressure distillation to obtain 4-trifluoromethylbenzylchloride. The preparation method for 4-trifluoromethylbenzyl chloride is simple in route and high in yield.

Description

technical field [0001] The invention relates to a preparation method of a compound, especially a preparation method of p-trifluoromethylbenzyl chloride. Background technique [0002] p-Trifluoromethylbenzyl chloride is an important organic synthesis intermediate in the pesticide and pharmaceutical industries, and is widely used in the pesticide, pharmaceutical and chemical industries. At present, although there are multiple industrial methods for synthesizing p-trifluoromethyl benzyl chloride, most of them have the defects of higher cost or lower efficiency. How to provide a kind of p-trifluoromethyl chloride with simple route and high production efficiency The preparation method of benzyl is a technical problem to be solved by those skilled in the art. Contents of the invention [0003] The technical problem to be solved by the present invention is to provide a method for preparing p-trifluoromethylbenzyl chloride with simple route and high yield. [0004] A kind of tec...

Claims

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Application Information

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IPC IPC(8): C07C29/38C07C33/46C07C17/16C07C22/04C07C17/383C07C29/80
CPCC07C17/16C07C17/383C07C29/38C07C29/80C07C33/46C07C22/04
Inventor 吴勇才
Owner 江苏万隆科技有限公司
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