HCID 71272633、化合物 → HCID 86694735、化合物
反応式
[CH3:1][C:2]1[C:3]([C:17]#[N:18])=[CH:4][C:5]2[N:9]=[CH:8][N:7]([CH:10]3[CH2:15][CH2:14][CH2:13][CH2:12][O:11]3)[C:6]=2[CH:16]=1>N.CO.[Ni]>[CH3:1][C:2]1[C:3]([CH2:17][NH2:18])=[CH:4][C:5]2[N:9]=[CH:8][N:7]([CH:10]3[CH2:15][CH2:14][CH2:13][CH2:12][O:11]3)[C:6]=2[CH:16]=1参加物
5
反応条件
- 温度
- 25 °C
実験手順
A suspension of 176 (4.6 g, 19 mmol) Raney-Ni (>15 eq) in 7N NH3 solution in MeOH (10 mL) was stirred under hydrogen at 25° C. for 2 h. The mixture was filtered and concentrated in vacuo. The crude product was purified by SiO2 chromatography eluting with a MeOH/DCM gradient (3 to 5% MeOH) to afford 3.2 g (69%) of (6-methyl-1-tetrahydropyran-2-yl-benzimidazol-5-yl)methanamine (178) as a yellow oil: MS (ESI) m/z=246 [M+1]+.
後処理
- filtrationThe mixture was filtered
- concentrationconcentrated in vacuo
- customThe crude product was purified by SiO2 chromatography
- washeluting with a MeOH/DCM gradient (3 to 5% MeOH)
出典と根拠
- ORDレコード
- ord-f558ac91a4ac4707844f0b051ff026d6
- 出典データセット
- uspto-grants-2014_01
- 特許番号
- US08637537B2
反応ノート
読み込み中…