Water → HCID 178457773、化合物
反応式
[Cl:1][C:2]1=[C:3]([Cl:9])[C:4]([O:6][C:7]1=[O:8])=[O:5].[CH3:10][CH:11]([CH2:14][C:15]1[CH:20]=[CH:19][C:18]([C:21]([CH3:24])([CH3:23])[CH3:22])=[CH:17][CH:16]=1)[CH2:12][NH2:13].O>C(O)(=O)C>[CH3:10][CH:11]([CH2:14][C:15]1[CH:16]=[CH:17][C:18]([C:21]([CH3:22])([CH3:24])[CH3:23])=[CH:19][CH:20]=1)[CH2:12][N:13]=[C:4]([OH:5])/[C:3](/[Cl:9])=[C:2](/[Cl:1])\[C:7]([OH:6])=[O:8]参加物
5
実験手順
16.7 g (0.1 mol) of dichloromaleic anhydride and 20.5 g (0.1 mol) of 2-methyl-3-(4-tert.-butylphenyl)-propylamine are stirred in 100 ml of glacial acetic acid under reflux for 4 hours. 100 ml of water are added, the oil which has separated out is extracted with methylene chloride, the methylene chloride phase is concentrated and the residue is recrystallized from ethanol. 14.6 g (41.2% of theory) of dichloromaleic acid N-[2-methyl-3-(4-tert.-butylphenyl)-propyl]-imide of melting point 64°-65° C. are obtained.
後処理
- temperatureunder reflux for 4 hours
- customthe oil which has separated out
- extractionis extracted with methylene chloride
- concentrationthe methylene chloride phase is concentrated
- customthe residue is recrystallized from ethanol
出典と根拠
- ORDレコード
- ord-0757c7d5569f4122929dde6c4dc20450
- 出典データセット
- uspto-grants-1986_04
- 特許番号
- US04582849
反応ノート
読み込み中…