Triethylamine → 2,2-difluoro-N-methoxy-N-methylcyclopropane-1-carboxamide
反応式
[F:1][C:2]1([F:8])[CH2:4][CH:3]1[C:5](Cl)=[O:6].FF.Cl.[CH3:12][NH:13][O:14][CH3:15].C(N(CC)CC)C>ClCCl.O>[F:1][C:2]1([F:8])[CH2:4][CH:3]1[C:5]([N:13]([O:14][CH3:15])[CH3:12])=[O:6]参加物
7
実験手順
7.00 g (49.8 mmol) of 2,2-difluorocyclopropanecarbonyl chloride (described in the Journal of Fluorine Chemistry 1990, 49, 127-139) in 100 ml of dichloromethane were mixed with 6.32 g (64.8 mmol) of N,O-dimethylhydroxylamine hydrochloride and 18.1 ml (130 mmol) of triethylamine and stirred at RT overnight. Water was added to the reaction mixture, the phases were separated, and the aqueous phase was extracted twice with dichloromethane. The combined organic phases were dried over sodium sulfate and concentrated. 5.73 g (70% of theory) of the title compound were obtained and were reacted without further purification.
後処理
- customthe phases were separated
- extractionthe aqueous phase was extracted twice with dichloromethane
- dry with materialThe combined organic phases were dried over sodium sulfate
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-481566167d8947818e363c2f0c197f81
- 出典データセット
- uspto-grants-2011_11
- 特許番号
- US08063234B2
反応ノート
読み込み中…
