Sulfuric Acid → HCID 20135952、化合物
反応式
[F:1][C:2]1([F:18])[C:7]([F:9])([F:8])[O:6][C:5]([F:11])([F:10])[C:4](F)(F)[N:3]1[C:14]([F:17])([F:16])[F:15].S(=O)(=O)=[O:20].S(=O)(=O)(O)O.FC1(F)OC(F)(F)C(=O)N(C(F)(F)F)C1=O>>[F:10][C:5]1([F:11])[O:6][C:7]([F:9])([F:8])[C:2]([F:18])([F:1])[N:3]([C:14]([F:17])([F:16])[F:15])[C:4]1=[O:20]参加物
5
反応条件
- 温度
- 25 °C
実験手順
To 253 g. (0.85 mol) of perfluoro-(N-methyl-morpholine) in a 300 ml. autoclave is added 72 g. (0.9 mol) of sulfur trioxide. The vessel is sealed, heated and rocked at 120° C. for 6 hrs. The autoclave is then cooled to 25° C., vented to release volatile materials and the residue charged to a 500 cc. flask equipped with magnetic stirrer, dropping funnel, condenser and thermometer. A solution of 195 g. of 96% sulfuric acid and 5 g. of H2C is added dropwise with stirring. The temperature is kept below 50° C. After the sulfuric acid is added the mixture is heated and stirred at reflux (55°-60° C.) for four hours. Distillation yields a large fraction, 207 g., b.p. 48°-65° C./740 mm., which consists of 45% by weight perfluoror-N-methyl-3-oxo-morpholine (40% conversion) and 15% by weight of higher boiling products believed to include perfluoro-(N-methyl-3,5dioxo-morpholine). Isolation of the pure amide (b.p. 59°-60° C./740 mm.) can be accomplished by distillation through a 25-plate column.