HCID 67264659、化合物 → HCID 67263426、化合物
反応式
[CH3:1][N:2]1[C:8]2[C:9]([N+:13]([O-])=O)=[CH:10][CH:11]=[CH:12][C:7]=2[C:6](=[O:16])[NH:5][CH2:4][CH2:3]1>CO.[Pd]>[NH2:13][C:9]1[C:8]2[N:2]([CH3:1])[CH2:3][CH2:4][NH:5][C:6](=[O:16])[C:7]=2[CH:12]=[CH:11][CH:10]=1参加物
4
実験手順
1-Methyl-9-nitro-1,2,3,4-tetrahydro-benzo[e][1,4]diazepin-5-one (#) (100 mg, 0.45 mmol) was dissolved in MeOH (20 ml) and placed in a Parr bottle. Pd—C (10%, 10 mg) was added, and the resulting mixture was shaken under 20 psi H2 for 1.5 h. The reaction mixture was filtered through celite, washed with MeOH, and concentrated to afford 9-Amino-1-methyl-1,2,3,4-tetrahydro-benzo[e][1,4]diazepin-5-one as a brown solid (86 mg, 99%). mp 130-133° C.; LCMS: m/z=192.30 (M+H+); 1H NMR (400 MHz, CDCl3) δ 7.26 (m, 1H), 6.80 (m, 2H), 3.79 (bs, 2H), 3.45 (m, 4H), 3.16 (s, 3H).
後処理
- filtrationThe reaction mixture was filtered through celite
- washwashed with MeOH
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-f877890695e645f68880a29f2a62720b
- 出典データセット
- uspto-grants-2012_04
- 特許番号
- US08148391B2
反応ノート
読み込み中…