2925-22-6Relevant articles and documents
Craig et al.
, p. 3572 (1971)
Van Eijck
, p. 1,3, 5, 8-10, 12 (1977)
Synthetic method of ethyl 4, 4-difluoro-3-oxo-2-piperidine-1-yl methylene butyrate
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Paragraph 0025; 0029; 0035; 0040; 0043; 0048; 0051; 0056, (2021/01/30)
The invention relates to a synthetic method of ethyl 4, 4-difluoro-3-oxo-2-piperidine-1-methylene butyrate. The synthetic method comprises the following steps: 1, carrying out a condensation reactionon difluoroacetyl fluoride and 3-(1-piperidyl)-ethyl acrylate to generate 4, 4-difluoro-3-oxo-2-piperidine-1-yl methylene ethyl butyrate and hydrogen fluoride, and 2, carrying out a reaction on the hydrogen fluoride generated in the step 1 and trichloroethylene under the action of a fluorination catalyst to generate trifluoroethylene and hydrogen chloride, and 3, reacting the trifluoroethylene generated in the step 2 with oxygen under the action of a complex catalyst to generate difluoroacetyl fluoride, and recycling the difluoroacetyl fluoride generated in the step 3 as a reactant in the step1. According to the synthetic method of the ethyl 4, 4-difluoro-3oxo-2-piperidine-1-methylene butyrate, the raw materials are simple and easy to obtain, the atom utilization rate is high, and the production safety is high.
Synthetic method of difluoroacetyl fluoride
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Paragraph 0041; 0045-0046; 0058; 0062-0063; 0066; 0070-0071, (2020/12/10)
The invention relates to a synthesis method of difluoroacetyl fluoride, which comprises the following steps: 1. reacting trichloroethylene with oxygen under the catalytic action of trialkyl boron shown in the formula I to generate dichloroacetyl chloride, and 2. reacting dichloroacetyl chloride with inorganic fluoride shown in the formula II under the action of a catalyst to generate difluoroacetyl fluoride. According to the synthetic method of difluoroacetyl fluoride, the raw materials are simple and easy to obtain, high-temperature reaction is not needed, and the yield is high.
Preparation method of 2,2-difluoroacetyl fluoride and derivative thereof
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Paragraph 0029-0046, (2017/07/21)
The invention belongs to the field of fluorine chemical industry and particularly relates to a preparation method of 2,2-difluoroacetyl fluoride and a derivative thereof. The preparation method takes 1,1,2,2-tetrafluoroethyl ethyl ether as a raw material, and the raw material reacts under the action of a catalyst to prepare the product. The catalyst is prepared by adopting a method comprising the following steps: taking rare-earth metal oxide as a raw material and activating at high temperature; and introducing CHF2Cl and reacting. The preparation method takes the 1,1,2,2-tetrafluoroethyl ethyl ether as the raw material, and the 1,1,2,2-tetrafluoroethyl ethyl ether has oxidization reaction under the action of the catalyst at 140 DEG C to 160 DEG C to generate acyl fluoride; and the preparation method has simple and safe production steps and short reaction time.