1-(6-fluoro-2H-chromen-4-yl)methanamine hydrochloride → (6-fluoro-3,4-dihydro-2H-1-benzopyran-4-yl)methanamine
반응식
Cl.[F:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[O:9][CH2:8][CH:7]=[C:6]2[CH2:13][NH2:14]>CO.CC(O)=O.[Ni]>[F:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[O:9][CH2:8][CH2:7][CH:6]2[CH2:13][NH2:14]참가 물질
5
실험 절차
To a solution of 1-(6-fluoro-2H-chromen-4-yl)methanamine hydrochloride (1.36 g, 7.6 mmol) in MeOH (20 mL) and AcOH (10 mL) was added Raney Nickel (760 mg) at room temperature. The suspension was stirred at rt overnight under 50 psi of H2. The reaction mixture was filtered and concentrated. The residue was dissolved in DCM and washed with sat. NaHCO3, dried (Na2SO4), and concentrated to give 490 mg (36%) of the title compound as a green oil. [M+H] calc'd for C10H12FNO, 182. Found 182.
후처리
- filtrationThe reaction mixture was filtered
- concentrationconcentrated
- dissolutionThe residue was dissolved in DCM
- washwashed with sat. NaHCO3
- dry with materialdried (Na2SO4)
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-58d6cd6702e246b7bdfa76bfdadeb4b6
- 출처 데이터셋
- uspto-grants-2015_02
- 특허 번호
- US08952151B2
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