Triethylamine → 2,2-difluoro-N-methoxy-N-methylcyclopropane-1-carboxamide
반응식
[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]참가 물질
7
실험 절차
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.
후처리
- customthe phases were separated
- extractionthe aqueous phase was extracted twice with dichloromethane
- dry with materialThe combined organic phases were dried over sodium sulfate
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-481566167d8947818e363c2f0c197f81
- 출처 데이터셋
- uspto-grants-2011_11
- 특허 번호
- US08063234B2
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