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Method for preparing 4,4-difluoro cyclohexanone diethyl acetal

A technology of difluorocyclohexanone ethylene diketal and cyclohexenone ethylene diketal, which is applied in the field of preparation 4, can solve problems such as uneconomical application and waste, and achieve production cost saving, simple process, and cheap and easy raw materials. The effect

Inactive Publication Date: 2012-07-04
SHANGHAI SINOFLUORO SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this way, a large amount of waste will be caused, which is uneconomical in industrial application and causes a large amount of waste.

Method used

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  • Method for preparing 4,4-difluoro cyclohexanone diethyl acetal
  • Method for preparing 4,4-difluoro cyclohexanone diethyl acetal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Under the protection of nitrogen, put 2 mol of 4-fluoro-3-cyclohexenone ethylene diketal (2) into the reaction bottle, add 2 mol of HF dropwise, after the dropwise addition, cool down to -30°C, add 0.2 mol of triethylamine dropwise , the dropwise addition time is 2h, react for 30h after the dropwise addition is completed, then pour the reaction solution into water, extract the water phase with dichloromethane after layering, spin dry and recrystallize, and prepare 4,4-difluorocyclohexane Ketone ethylene diketal 1.6mol, the yield is 80%.

Embodiment 2

[0016] Under the protection of nitrogen, put 1 mol of 4-fluoro-3-cyclohexenone ethylene diketal (2) into the reaction bottle, add 1 mol of HF dropwise, after the dropwise addition, cool down to -20°C, add 0.1 mol of triethylamine dropwise , the dropwise addition time is 2h, react for 36h after the dropwise addition is completed, then pour the reaction liquid into water, extract the water phase with dichloromethane after layering, spin dry and recrystallize, and prepare 4,4-difluorocyclohexane Ketone ethylene diketal (1) 0.7, the yield is 70%.

Embodiment 3

[0018] Under the protection of nitrogen, put 2 mol of 4-fluoro-3-cyclohexenone ethylene diketal (2) into the reaction bottle, add 2 mol of HF dropwise, after the dropwise addition, cool down to -40°C, add 0.2 mol of triethylamine dropwise , the dropping time is 2 hours, and the reaction is 24 hours after the dropping is completed. Subsequently, the reaction solution is poured into water, and the water phase is extracted with dichloromethane after layering. After spinning to dryness and recrystallization, the 4,4-difluorocyclic Hexanone ethylene diketal (1) 1.7mol, the yield is 85%.

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Abstract

The invention provides a method for preparing 4,4-difluoro cyclohexanone diethyl acetal, which is characterized by comprising the following steps: putting 4-fluorine-3-cyclohexenone diethyl acetal (2) into a reaction flask; dripping hydrogen fluoride (HF); after the HF is dripped, cooling to -20--40DEG C; dripping triethylamine; reacting for 26-36 hours; pouring reaction solution into water; after layering, extracting an aqueous phase with dichloromethane; and after spin dry and recrystallization, preparing to obtain the 4,4-difluoro cyclohexanone diethyl acetal (1), wherein a reaction formula is disclosed as follows. Compared with the prior art, the method for preparing the 4,4-difluoro cyclohexanone diethyl acetal has the beneficial effects of simple technology, the 4-fluorine-3-cyclohexenone diethyl acetal can be reused, and the production cost is saved.

Description

field of invention [0001] The invention relates to a method for preparing 4,4-difluorocyclohexanone ethylene diketal. Background technique [0002] Most of the existing fluorination reactions use fluorinating reagents, and difluorocyclohexanone is a hot spot in new drug research. [0003] At present, when diethylamine sulfur trifluoride (DAST) is used for fluorination, half of the product is 4-fluoro-3-cyclohexenone ethylene diketal, which is currently treated as waste. Like this, will cause a large amount of wastes, be uneconomical in the application of industry, cause a large amount of wastes. Therefore, there is a need for a synthetic method that can reuse 4,4-difluorocyclohexanone, thereby allowing diethylamine sulfur trifluoride (DAST) to be more economical in the production of fluorinated applications. sex. Contents of the invention [0004] The object of the present invention is to provide a kind of method for preparing 4,4-difluorocyclohexanone ethylene diketal,...

Claims

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Application Information

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IPC IPC(8): C07D317/72
Inventor 柳叶闾肖波
Owner SHANGHAI SINOFLUORO SCI
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