Cumene → (S)-1-benzyl-3-hydroxypyrrolidine-2,5-dione
反応式
[C:1]([OH:9])(=O)[C@H:2]([CH2:4][C:5](O)=[O:6])[OH:3].[CH2:10]([NH2:17])[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.C1(C(C)C)C=CC=CC=1>O>[CH2:10]([N:17]1[C:5](=[O:6])[CH2:4][C@H:2]([OH:3])[C:1]1=[O:9])[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1参加物
5
実験手順
A mixture of 50.0 g (0.373 mole) (S)-malic acid (Ia), 41 ml (0.373 mole) benzyl amine and 250 ml cumene was heated with an internal temperature of 155° C. for 2.5 h on a water separator, during which time 12 ml water were separated. An oily phase formed during cooling off which slowly crystallized. The cumene was decanted off thereafter and the residue crystallized out of 220 ml EtOH. 30.3 g (39.6%) (S)-1-benzyl-3-hydroxy-2,5-pyrrolidinedione (IIa) were isolated in the form of colorless crystals.
後処理
- customwere separated
- customAn oily phase formed
- temperatureduring cooling off which
- customslowly crystallized
- customThe cumene was decanted off
- customthe residue crystallized out of 220 ml EtOH
出典と根拠
- ORDレコード
- ord-b610e96e4bf14fa2b45f8c820a93921d
- 出典データセット
- uspto-grants-1996_12
- 特許番号
- US05585500
反応ノート
読み込み中…