Triethylamine → tert-Butyl (2-oxo-3-pyrimidin-4-yl-2,3-dihydro-1H-benzimidazol-1-yl)acetate
反応式
[C:1]([O:5][C:6](=[O:25])[CH2:7][N:8]1[C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][C:11]=2[N:10]([C:17]2[CH:22]=[C:21](Cl)[N:20]=[CH:19][N:18]=2)[C:9]1=[O:24])([CH3:4])([CH3:3])[CH3:2].C(N(CC)CC)C>CCO.[Pd]>[O:24]=[C:9]1[N:8]([CH2:7][C:6]([O:5][C:1]([CH3:4])([CH3:3])[CH3:2])=[O:25])[C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][C:11]=2[N:10]1[C:17]1[CH:22]=[CH:21][N:20]=[CH:19][N:18]=1参加物
5
実験手順
A mixture of tert-butyl[3-(6-chloropyrimidin-4-yl)-2-oxo-2,3-dihydro-1H-benzimidazol-1-yl]acetate from Step A (260 mg, 0.720 mmol), 10% Pd/C (23 mg) and triethylamine (0.150 mL, 1.08 mmol) in EtOH (5 mL) was stirred under an atmosphere of hydrogen (ca. 1 atm) for 2 h. The mixture was filtered through a pad of Celite, washing with EtOH, and the filtrate was concentrated to give the title compound. MS: m/z=327 (M+1).
後処理
- filtrationThe mixture was filtered through a pad of Celite
- washwashing with EtOH
- concentrationthe filtrate was concentrated
出典と根拠
- ORDレコード
- ord-a6754c131c6f409bb7b991b59fcd3016
- 出典データセット
- uspto-grants-2011_08
- 特許番号
- US08003792B2
反応ノート
読み込み中…