2-(3,5-dimethyl-4-nitro-1H-pyrazol-1-yl)ethanol → HCID 28492268、化合物
反応式
[CH3:1][C:2]1[C:6]([N+:7]([O-])=O)=[C:5]([CH3:10])[N:4]([CH2:11][CH2:12][OH:13])[N:3]=1>CCOC(C)=O.CCO.O=[Pt]=O>[NH2:7][C:6]1[C:2]([CH3:1])=[N:3][N:4]([CH2:11][CH2:12][OH:13])[C:5]=1[CH3:10]参加物
5
実験手順
To a solution of 2-(3,5-dimethyl-4-nitro-1H-pyrazol-1-yl)ethanol (624 mg, 3.37 mmol) in EtOAc (1.2 mL, degassed) and EtOH (3.6 mL, degassed), PtO2 (66 mg, 0.34 mmol) was added and the reaction mixture was stirred at rt under a H2-atmosphere for 30 h. The mixture was diluted with EtOH, filtered over celite and the filter cake was rinsed with EtOH. The filtrate was concentrated to obtain 2-(4-amino-3,5-dimethyl-1H-pyrazol-1-yl)ethanol as a pale brown solid, which was used in the next step without further purification. LC-MS conditions A: tR=0.16 min, [M+H]+=156.29.
後処理
- filtrationfiltered over celite
- washthe filter cake was rinsed with EtOH
- concentrationThe filtrate was concentrated
出典と根拠
- ORDレコード
- ord-64b539c5722544fe886d95e3c08f3fba
- 出典データセット
- uspto-grants-2016_04
- 特許番号
- US09303023B2
反応ノート
読み込み中…