2-(4-Nitro-1H-pyrazol-1-yl)ethan-1-ol → 2-(4-Amino-1H-pyrazol-1-yl)ethanol
反応式
[N+:1]([C:4]1[CH:5]=[N:6][N:7]([CH2:9][CH2:10][OH:11])[CH:8]=1)([O-])=O>CO.[Pd]>[NH2:1][C:4]1[CH:5]=[N:6][N:7]([CH2:9][CH2:10][OH:11])[CH:8]=1参加物
4
実験手順
A solution of 2-(4-nitro-1H-pyrazol-1-yl)ethanol (1.08 g, 6.87 mmol) in methanol (34 ml) was evacuated and purged with nitrogen and treated with palladium on carbon (0.1 g, 0.094 mmol). The resulting black suspension was evacuated and purged with a hydrogen balloon and stirred under hydrogen overnight. The mixture was filtered through celite with methanol washes, and concentrated. The residue was flash chromatographed (50 mm; 9% methanol/methylene chloride w/0.1% NH4OH then 10% methanol/methylene chloride w/0.1% NH4OH) to afford the title compound.
後処理
- custompurged with nitrogen
- customThe resulting black suspension was evacuated
- custompurged with a hydrogen balloon
- filtrationThe mixture was filtered through celite with methanol washes
- concentrationconcentrated
- customchromatographed (50 mm
出典と根拠
- ORDレコード
- ord-2a0a196daeb74c7eb9b5aced72273814
- 出典データセット
- uspto-grants-2013_04
- 特許番号
- US08426408B2
反応ノート
読み込み中…