- Method for co-producing 2-fluoropropionate and ethyl difluoroacetate
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The invention discloses a method for co-producing 2-fluoropropionate and ethyl difluoroacetate. The method comprises: (a) carrying out a reaction on a fluorinating reagent and a lactate for 0.5-7 h ata reaction temperature of 30-120 DEG C according to a molar ratio of 0.5-2:1, cooling the reaction material after completing the reaction, adding a nitrogen-containing compound, and carrying out pressure reducing rectification to obtain a 2-fluoropropionate product and N,N-dimethyl difluoroacetamide; and (b) adding concentrated sulfuric acid to a mixture of anhydrous ethanol and the N,N-dimethyldifluoroacetamide obtained in the step (a), carrying out a reaction for 1-10 h at a reaction temperature of 50-170 DEG C, cooling after completing the reaction, separating the liquid, and carrying outrectification to obtain the ethyl difluoroacetate product, wherein a molar ratio of anhydrous ethanol to N,N-dimethyl difluoroacetamide is 0.5-4.5:1, and a molar ratio of concentrated sulfuric acid to N,N-dimethyl difluoroacetamide is 0.1-1.5:1. According to the present invention, the method has advantages of environmental protection, high yield and low cost.
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Paragraph 0035; 0036
(2019/05/04)
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- Reactions of 1,1,2,2-tetrafluoroethyl-N,N-dimethylamine with linear and cyclic 1,3-diketones
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Ketones are known to be unreactive toward α-fluoroamines such as Ishikawa's Reagent or 1,1,2,2-tetrafluoroethyl-N,N-dimethylamine (TFEDMA). On the other hand, 1,3-diketones were found to undergo fluorination with TFEDMA. In the case of linear 1,3-diketone
- Grieco, Liane M.,Halliday, Gary A.,Junk, Christopher P.,Lustig, Steven R.,Marshall, William J.,Petrov, Viacheslav A.
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experimental part
p. 1198 - 1206
(2011/12/01)
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- STEREOSELECTIVE ONE STEP FLUORINATION PROCESS FOR THE PREPARATION OF 2-FLUOROPROPIONATE
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The current invention describes a one-step process for the synthesis of 2-fluoropropionates from lactic acid ester derivatives using TFEDMA.
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Page/Page column 6
(2008/12/05)
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- 1,1,2,2-Tetrafluoroethyl-N,N-dimethylamine: A new selective fluorinating agent
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The title compound has been prepared in 96-98% yield by the reaction of tetrafluoroethylene and dimethylamine. 1,1,2,2-Tetrafluoroethyl-N,N-dimethylamine (1) is found to be an effective reagent for the conversion of alcohols into alkyl fluorides. Reaction of 1 and primary alcohols proceeds with high yield formation of the corresponding alkyl fluorides at elevated temperature. However, the reaction of secondary and tertiary alcohols rapidly takes place at 0-10°C, producing corresponding alkyl fluorides as major product along with some olefins.
- Petrov,Swearingen,Hong,Chris Petersen
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