Triethylamine → 2,2-Difluoroethyl trifluoromethanesulfonate
反応式
S([O:8][S:9]([C:12]([F:15])([F:14])[F:13])(=[O:11])=[O:10])(C(F)(F)F)(=O)=O.[F:16][CH:17]([F:20])[CH2:18]O.C(N(CC)CC)C>ClCCl>[F:16][CH:17]([F:20])[CH2:18][O:8][S:9]([C:12]([F:13])([F:14])[F:15])(=[O:11])=[O:10]参加物
5
反応条件
- 温度
- 25 °C
実験手順
In a flask under argon was placed triflic anhydride (10.22 mL, 61 mmol) and dichloromethane (10 mL) and it was cooled to −70° C. To this cooled mixture was added slowly a solution of 2,2-difluoroethanol (5.00 g, 61 mmol) and triethylamine (8.5 mL, 61 mmol) in dichloromethane (10 mL). After the addition was complete, the mixture was warmed to 25° C. and then concentrated in vacuo. This material was distilled at 60° C. and 50 mm Hg which afforded trifluoro-methanesulfonic acid 2,2-difluoro-ethyl ester (9.74 g, 75%) as a colorless oil.
後処理
- customIn a flask under argon was placed
- additionAfter the addition
- concentrationconcentrated in vacuo
- distillationThis material was distilled at 60° C.
出典と根拠
- ORDレコード
- ord-7ce4d0728fee45208e0af46ba190a52b
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07741327B2
反応ノート
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