Methylhydrazine → 3-Isopropyl-1-methyl-1H-pyrazol-5-amine
反応式
[CH3:1][CH:2]([CH3:9])[C:3](=C=O)[CH2:4][C:5]#[N:6].[CH3:10][NH:11][NH2:12]>>[CH3:10][N:11]1[C:5]([NH2:6])=[CH:4][C:3]([CH:2]([CH3:1])[CH3:9])=[N:12]1参加物
3
実験手順
Under nitrogen atmosphere, the compound of Example 2A (8.03 g, 72 mmol) was dissolved in alcohol (50 mL). Methylhydrazine (3.32 g, 72 mmol) was added. The resultant mixture was slowly warmed and refluxed with stirring. The reaction was kept for 3 hr. The reaction was stopped and cooled to room temperature. Alcohol was rotary-evaporated to obtain a crude product as oil. The crude product was purified with column chromatography (eluant: petroleum ether/ethyl acetate=1:1) to give 5.2 g of the title compound. MS (ESI): m/z 140 (M+H)+
後処理
- temperaturerefluxed
- customAlcohol was rotary-evaporated
- customto obtain a crude product as oil
- customThe crude product was purified with column chromatography (eluant: petroleum ether/ethyl acetate=1:1)
出典と根拠
- ORDレコード
- ord-b0a427dbb42b4f299a59db135276713d
- 出典データセット
- uspto-grants-2016_02
- 特許番号
- US09249172B2
反応ノート
読み込み中…