Sulfur trioxide → Difluoromalonyl fluoride

HRID 1680420

反応式

HRID 1680420 の反応式
C[O:2][C:3](F)([F:10])[C:4]([F:9])([F:8])[C:5]([F:7])=[O:6].S(=O)(=O)=O>>[F:8][C:4]([F:9])([C:5]([F:7])=[O:6])[C:3]([F:10])=[O:2]

参加物

3

反応物 2

HCID 24682Sulfur trioxideHCID 136846932,2,3,3-Tetrafluoro-3-methoxypropanoyl fluoride

生成物 1

HCID 2774099Difluoromalonyl fluoride

実験手順

3-Methoxytetrafluoropropionyl fluoride (F. S. Fawcett, C. W. Tullock and D. D. Coffman, J. Amer. Chem. Soc., 84, 4275 (1962)) (81 g, 0.45 mol) was slowly added to sulfur trioxide (80 g, 1.0 mol) at 40° C., and the product difluoromalonyl difluoride, bp -9° C., was continuously removed by distillation through a low temperature still, yield 58 g (0.40 mol, 90%). The product structure was confirmed by: λmax 1860 cm-1 (COF), 19F NMR (no solvent), +17.1 ppm (t J=10 Hz), 2F, COF and -114.2 ppm (t J=10 Hz) 2F, CF2.

後処理

  1. customthe product difluoromalonyl difluoride, bp -9° C., was continuously removed by distillation through a low temperature still

出典と根拠

ORDレコード
ord-325d9b4ab01649eb8e2c2eedd0c4cd92
出典データセット
uspto-grants-1981_06
特許番号
US04273729

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