Hydrazine hydrate (1:1) → 1-(2-Hydrazinopyridin-4-yl)ethanol
反応式
Cl[C:2]1[CH:7]=[C:6]([CH:8]([OH:10])[CH3:9])[CH:5]=[CH:4][N:3]=1.O.[NH2:12][NH2:13]>CO.CCOCC>[NH:12]([C:2]1[CH:7]=[C:6]([CH:8]([OH:10])[CH3:9])[CH:5]=[CH:4][N:3]=1)[NH2:13]参加物
5
反応条件
- 温度
- 100 °C
実験手順
1-(2-chloropyridin-4-yl)ethanol (5d) (14.3 g) was dissolved in hydrazine hydrate (275 mL). The resulting mixture was heated at 100° C. with stirring overnight. The mixture was concentrated under vacuum to give a yellow oil that was dissolved in a small volume of methanol and ether was added, which resulted in precipitation of a white solid. The obtained suspension was stirred for 30 minutes and filtered, and the residue (hydrazine hydrochloride) was discarded. The filtrate was concentrated under vacuum to give the title compound (13.7 g) as a light-brown oil.
後処理
- concentrationThe mixture was concentrated under vacuum
- customto give a yellow oil that
- additionwas added
- customwhich resulted in precipitation of a white solid
- stirringThe obtained suspension was stirred for 30 minutes
- filtrationfiltered
- concentrationThe filtrate was concentrated under vacuum
出典と根拠
- ORDレコード
- ord-f10144315593443384fb8eac4ba5b9ee
- 出典データセット
- uspto-grants-2015_02
- 特許番号
- US08952001B2
反応ノート
読み込み中…