Hydrazine hydrate (1:1) → HCID 86724908、化合物
反応式
[CH:1]([N:4]1[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[C:6]([C:13]([O:15]C)=O)=[N:5]1)([CH3:3])[CH3:2].O.[NH2:18][NH2:19]>C(O)C>[CH:1]([N:4]1[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[C:6]([C:13]([NH:18][NH2:19])=[O:15])=[N:5]1)([CH3:3])[CH3:2]参加物
4
実験手順
To a stirred solution of methyl 1-isopropyl-1H-indazol-3-yl carboxylate (40.0 grams, 183.5 mmol, obtained in above step) in ethanol at room temperature hydrazine hydrate (130 mL, 2.56 mmol) was added. The reaction mixture was refluxed for 2 hours. The volatiles were removed under reduced pressure and the crude mass was diluted with dichloromethane, washed with water, brine, dried over anhydrous sodium sulphate and the solvent was removed under reduced pressure to obtain the title compound (37.52 grams).
後処理
- temperatureThe reaction mixture was refluxed for 2 hours
- customThe volatiles were removed under reduced pressure
- additionthe crude mass was diluted with dichloromethane
- washwashed with water, brine
- dry with materialdried over anhydrous sodium sulphate
- customthe solvent was removed under reduced pressure
出典と根拠
- ORDレコード
- ord-4dfb8bb93adf48499c73af397eb0ecc4
- 出典データセット
- uspto-grants-2015_07
- 特許番号
- US09079894B2
反応ノート
読み込み中…