p-Toluenesulfonic acid → (5S)-5-(Hydroxymethyl)-3,3-dimethylpyrrolidin-2-one
反応式
CC1(C)[N:6]2[C:7](=[O:12])[C:8]([CH3:11])([CH3:10])[CH2:9][CH:5]2[CH2:4][O:3]1.C1(C)C=CC(S(O)(=O)=O)=CC=1>CO>[OH:3][CH2:4][C@H:5]1[NH:6][C:7](=[O:12])[C:8]([CH3:11])([CH3:10])[CH2:9]1参加物
4
実験手順
A mixture of 27.15 g I.46 (3,3,6,6-tetramethyl-tetrahydro-pyrrolo[1,2-c]oxazol-5-one) and 0.282 g p-toluenesulfonic acid in 500 ml methanol was stirred at reflux overnight. The mixture was concentrated. Additional 500 ml methanol and 2.8 g p-toluenesulfonic acid were added and the mixture was stirred 4 h at reflux. The mixture was diluted with water and treated with sodium carbonate to obtain a basic pH. The organic layer was separated, dried with magnesium sulfate and concentrated to give 1 g (60% content; 3% of theory)
後処理
- temperatureat reflux overnight
- concentrationThe mixture was concentrated
- additionAdditional 500 ml methanol and 2.8 g p-toluenesulfonic acid were added
- stirringthe mixture was stirred 4 h
- temperatureat reflux
- additionThe mixture was diluted with water
- additiontreated with sodium carbonate
- customto obtain a basic pH
- customThe organic layer was separated
- dry with materialdried with magnesium sulfate
- concentrationconcentrated
- customto give 1 g (60% content; 3% of theory)
出典と根拠
- ORDレコード
- ord-ea77c2c9eb9b41fc9f6c1748de399bca
- 出典データセット
- uspto-grants-2014_07
- 特許番号
- US08772305B2
反応ノート
読み込み中…