Borane;tetrahydrofuran → [(3-Bromo-4-fluorophenyl)methyl](methyl)amine
반응식
C[C:2]([N:5]([CH2:9][C:10]1[CH:15]=[CH:14][C:13]([F:16])=[C:12]([Br:17])[CH:11]=1)C(=O)[O-])(C)C.B.C1COCC1>C1COCC1>[Br:17][C:12]1[CH:11]=[C:10]([CH2:9][NH:5][CH3:2])[CH:15]=[CH:14][C:13]=1[F:16]참가 물질
4
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- 온도
- 80 °C
실험 절차
To the solution of 1,1-dimethylethyl[(3-bromo-4-fluorophenyl)methyl]carbamate (0.755 g, 2.48 mmol) in THF (1 mL) was added BH3.THF (12.5 mL, 1.0 M in THF). The mixture was heated in a microwave machine at about 80° C. for about 30 mins twice. The reaction was then quenched with HCl (10 mL, 1 N) slowly, stirred for 2 h at room temperature, basified with NaHCO3 to pH ˜9, and extracted with EtOAc (50+20 mL). The organic layer was washed with brine, dried over Na2SO4, filtered, concentrated to afford 0.52 g (96%) of the title compound. LC-MS m/z 218 (M+H)+.
후처리
- customThe reaction was then quenched with HCl (10 mL, 1 N) slowly
- extractionextracted with EtOAc (50+20 mL)
- washThe organic layer was washed with brine
- dry with materialdried over Na2SO4
- filtrationfiltered
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-a6df705ab80d4a47923871b64a16cd65
- 출처 데이터셋
- uspto-grants-2011_12
- 특허 번호
- US08071588B2
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