Water → 2-Bromo-6-(difluoromethoxy)pyridin-3-amine
반응식
[F:1][CH:2]([F:11])[O:3][C:4]1[N:9]=[CH:8][C:7]([NH2:10])=[CH:6][CH:5]=1.[Br:12]N1C(=O)CCC1=O.O>C(#N)C>[Br:12][C:8]1[C:7]([NH2:10])=[CH:6][CH:5]=[C:4]([O:3][CH:2]([F:1])[F:11])[N:9]=1참가 물질
5
실험 절차
6-Difluoromethoxy-pyridin-3-yl-amine obtained in Step B (1.36 g) was treated with N-bromosuccinimide (1.51 g) in acetonitrile for 10 minutes. The solution was poured into water, extracted with ethyl acetate, the organic layer dried over sodium sulfate and concentrated in vacuo. Chromatography on silica gel (eluent: cyclohexane/ethyl acetate 7:3) afforded 2-bromo-6-difluoromethoxy-pyridin-3-yl-amine as a red oil. 1H NMR (400 MHz, CDCl3) 3.95 (br s, 2H), 6.72 (d, 1H), 7.07 (d, 1H), 7.24 (dd, 1H).
후처리
- extractionextracted with ethyl acetate
- dry with materialthe organic layer dried over sodium sulfate
- concentrationconcentrated in vacuo
출처 및 근거
- ORD 기록
- ord-be65913758514361a2ac17f6149c502b
- 출처 데이터셋
- uspto-grants-2013_11
- 특허 번호
- US08586593B2
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