Phenylhydrazine → 5-Methyl-2-phenyl-3-pyrzolidinone
反応式
[C:1]([OH:6])(=O)/[CH:2]=[CH:3]/[CH3:4].[C:7]1([NH:13][NH2:14])[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1>CCOCC>[CH3:4][CH:3]1[CH2:2][C:1](=[O:6])[N:13]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)[NH:14]1参加物
4
反応条件
- 温度
- 155 °C
実験手順
17.2 g of crotonic acid (MW 86.09, 0.2 mol) was added to 21.6 g of phenylhydrazine (MW 108.14, 0.2 mol), and the mixture was stirred for one hour while heating at 150-160° C. The reaction solution was dissolved in 500 ml of ether. The solution was washed twice with 100 ml of 10% aqueous solution of sodium hydroxide and once with 100 ml of water, followed by evaporation of the ether. The resulting solid was dried under reduced pressure and recrystallized from toluene to obtain 20.31 g of 3-methyl-1-phenyl-5-pyrazolidone (MW 176.0, 0.126 mol, 58%).
後処理
- washThe solution was washed twice with 100 ml of 10% aqueous solution of sodium hydroxide and once with 100 ml of water
- customfollowed by evaporation of the ether
- customThe resulting solid was dried under reduced pressure
- customrecrystallized from toluene
出典と根拠
- ORDレコード
- ord-7a7bd770b2c94f6f8837212e7ee42c9c
- 出典データセット
- uspto-grants-2000_09
- 特許番号
- US06121305
反応ノート
読み込み中…