Hydrochloric Acid → 3-(5-Amino-3-tert-butyl-pyrazol-1-yl)-propan-1-ol
反応式
[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]=1参加物
5
実験手順
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+].
後処理
- temperaturethe reaction mixture was heated
- temperatureat reflux for 18 h
- concentrationThe mixture was concentrated in vacuo
- customthe residue was purified by FCC
出典と根拠
- ORDレコード
- ord-180bbe1933cb45b2ba248db74374a3b5
- 出典データセット
- uspto-grants-2015_05
- 特許番号
- US09029373B2
反応ノート
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