2366-56-5Relevant articles and documents
Method for co-producing 2-fluoropropionate and ethyl difluoroacetate
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Paragraph 0035; 0036, (2019/05/04)
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.
Method for preparing a fluorinated organic compound
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Paragraph 0293-0294, (2014/06/11)
A method for preparing a fluorinated organic compound (II) from an organic compound (I) comprising at least one nucleofugal group Nu, and also a preparation of different specific organic compounds, in particular a fluoro-methylpyrazole compound. The method comprises: a reaction, in the presence of water, of the organic compound (I) and at least one salt providing at least one fluoride anion; and a replacement of at least one nucleofugal group Nu of the compound (I) with a fluorine atom, in order to obtain the fluorinated organic compound (II).
Conformational analysis. Part 33. An NMR, solvation and theoretical investigation of conformational isomerism in N,N-dimethylfluoroacetamide and N,N-dimethyl-α-fluoropropionamide
Tormena, Claudio F.,Rittner, Roberto,Abraham, Raymond J.,Basso, Ernani A.,Pontes, Rodrigo M.
, p. 2054 - 2059 (2007/10/03)
The solvent and temperature dependence of the 1H and 13C NMR spectra of N,N-dimethylfluoroacetamide (DMFA) and N,N-dimethyl-α-fluoropropionamide (DMFP) are reported and the 5JCF, 1JCF and 4JCF couplings analysed by solvation theory. Density function theory (DFT) at the B3LYP/6-311 +G(d,p) level with ZPE (zero point energy) corrections was used to obtain the conformer geometries. In DMFA, the DFT method gave only two minima for the cis (F-C-C=O, 0°) and gauche (F-C-C=O, 140.6°) rotamers. The trans rotamer was not a minimum in the energy surface. Assuming only the cis and gauche forms, the observed couplings when analysed by solvation theory gave the energy difference (Ecis - Eg) of 2.5 kcal mol-1 in the vapour phase, (cf. the ab initio value of 2.3 kcal mol-1) decreasing to 0.87 kcal mol-1 in CCl4 and to -1.29 kcal mol-1 in DMSO. In DMFP the ab initio calculations gave three minima; the cis (F-C-C=O, 30.4°), gauche-1 (F-C-C=O, 144.7°) and gauche-2 (F-C-C=O, -124.1°) rotamers with (Ecis - Eg2) equal to 2.5 kcal mol-1 and (Eg1 - Eg2) equal to 0.3 kcal mol-1. The observed couplings were analysed by solvation theory assuming one "average" gauche conformer to give (Ecis - Eg(AV)) equal to 2.1 kcal mol-1 in the vapour phase, decreasing to 0.83 kcal mol-1 in CCl4 and to -1.11 kcal mol-1 in DMSO.
