Hydrochloric Acid → 3-(5-Amino-3-tert-butyl-pyrazol-1-yl)-propan-1-ol
반응식
[CH3:1][C:2]([CH3:9])([CH3:8])[C:3](=O)[CH2:4][C:5]#[N:6].Cl.Cl.[NH:12]([CH2:14][CH2:15][CH2:16][OH:17])[NH2:13].Cl>C(O)C>[NH2:6][C:5]1[N:12]([CH2:14][CH2:15][CH2:16][OH:17])[N:13]=[C:3]([C:2]([CH3:9])([CH3:8])[CH3:1])[CH:4]=1참가 물질
5
실험 절차
A solution of 4,4-dimethyl-3-oxo-pentanenitrile (0.7 g, 5.58 mmol) in ethanol (IMS grade, 5 mL) was treated with 3-hydrazino-propan-1-ol dihydrochloride (1 g, 6.13 mmol), followed by conc. HCl (0.05 mL), and the reaction mixture was heated at reflux for 18 h. The mixture was concentrated in vacuo and the residue was purified by FCC, using 0-10% [2M NH3 in MeOH] in DCM to afford the title compound as a white gummy solid (0.94 g, 85%). LCMS (Method 3): Rt 0.42 min, m/z 198 [MH+].
후처리
- temperaturethe reaction mixture was heated
- temperatureat reflux for 18 h
- concentrationThe mixture was concentrated in vacuo
- customthe residue was purified by FCC
출처 및 근거
- ORD 기록
- ord-180bbe1933cb45b2ba248db74374a3b5
- 출처 데이터셋
- uspto-grants-2015_05
- 특허 번호
- US09029373B2
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