Methylamine → (S)-(+)-Mandelamide
反応式
C[NH2:2].[C:3]([O:13]C)(=O)[C@H:4]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)[OH:5]>>[C:3]([NH2:2])(=[O:13])[C@H:4]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)[OH:5]参加物
3
実験手順
To a solution of methylamine (40% in water, 3.8 equivalents) is added, at ambient temperature, methyl (S)-mandelate (1.0 equivalent; commercially available), while keeping the temperature below 30° C. and stirred at ambient temperature until full conversion is achieved. Excess methylamine is removed by azeotropic distillation. Alternatively, after neutralisation with aqueous hydrochloric acid the aqueous solution is saturated with sodium chloride and extracted several times with dichloromethane. The organic layers are combined and the water is removed by azeotropic distillation.
後処理
- customthe temperature below 30° C.
- customExcess methylamine is removed by azeotropic distillation
- extractionextracted several times with dichloromethane
- customthe water is removed by azeotropic distillation
出典と根拠
- ORDレコード
- ord-6cc76b3a6a9943eca6dc37b5e07b6955
- 出典データセット
- uspto-grants-2012_08
- 特許番号
- US08247560B2
反応ノート
読み込み中…