Synthetic Route of 454-31-9, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 454-31-9, name is Ethyl 2,2-difluoroacetate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.
EXAMPLE 8 Ethyl 3,5-bis(difluoromethyl)-1H-pyrazole-4-carboxylate (Ia/b-3) To a mixture of (3.44 g, 10 mmol) ethyl 3-[(diphenylmethylene)hydrazinylidene]-4,4-difluorobutanoate and 1.02 g of ethyl difluoroacetate in 15 ml of methyl tert-butyl ether are added 1 g of potassium tert-butoxide and the mixture is stirred for 18 hours at 40 C. The mixture is cooled to 20 C., the precipitate is filtered off and dissolved in 15 ml of ethanol 2 ml of HCl were added to the solution and the mixture is stirred for 3 hours at 50 C. The product is extracted with 50 ml of methyl tert-butyl ether. The organic phase is washed with water, dried over MgSO4 and concentrated under reduced pressure. The residue is purified by means of column chromatography (ethyl acetate/methylcyclohexane). 1.87 g (78%) of product is obtained. 1NMR delta: 7.15 (t, 2h, CHF2, JH-F=53.6 Hz), 4.39 (q, 2H, CH2, J=7.1 Hz), 1.39 (t, 3H, CH3, J=7.1 Hz) ppm. 13C NMR delta: 161.1 (CO), 143.8 (t, CIV arom, JC-F=23.1 Hz), 111.6 (CIV arom), 108.2 (t, JC-F=238.4 Hz), 61.7 (CH2), 13.9 (CH3) ppm. 19F NMR delta: -117.3 (CHF2, JF-H=53.6 Hz) ppm.
The synthetic route of Ethyl 2,2-difluoroacetate has been constantly updated, and we look forward to future research findings.
Reference:
Patent; BAYER CROPSCIENCE AKTIENGESELLSCHAFT; PAZENOK, Sergii; LUI, Norbert; (10 pag.)US2016/122304; (2016); A1;,
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