1-(6-fluoro-2H-chromen-4-yl)methanamine hydrochloride → (6-fluoro-3,4-dihydro-2H-1-benzopyran-4-yl)methanamine
反応式
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]参加物
5
実験手順
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.
後処理
- filtrationThe reaction mixture was filtered
- concentrationconcentrated
- dissolutionThe residue was dissolved in DCM
- washwashed with sat. NaHCO3
- dry with materialdried (Na2SO4)
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-805485f5ee074f61a3cf7a7aa66ac45f
- 出典データセット
- uspto-grants-2015_07
- 特許番号
- US09085534B2
反応ノート
読み込み中…