HCID 71272633, 화합물 → HCID 86694735, 화합물
반응식
[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]=1참가 물질
5
반응 조건
- 온도
- 25 °C
실험 절차
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]+.
후처리
- 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)
출처 및 근거
- ORD 기록
- ord-f558ac91a4ac4707844f0b051ff026d6
- 출처 데이터셋
- uspto-grants-2014_01
- 특허 번호
- US08637537B2
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