Monobasic potassium phosphate → HCID 7091053、化合物
反応式
C([O:3][C:4](=[O:16])[CH2:5][CH:6]([NH2:15])[C:7]1[CH:12]=[C:11]([F:13])[CH:10]=[CH:9][C:8]=1[F:14])C.P([O-])(O)(O)=O.[K+]>O>[NH2:15][C@H:6]([C:7]1[CH:12]=[C:11]([F:13])[CH:10]=[CH:9][C:8]=1[F:14])[CH2:5][C:4]([OH:16])=[O:3]参加物
4
実験手順
3-Amino-3-(2,5-difluorophenyl)propionic acid ethyl ester (3 g) was emulsified in water (pH=9.2) and admixed with potassium dihydrogenphosphate (5 mg) (pH=8.5). After addition of Amano Lipase PS (150 mg), the mixture was stirred overnight. The pH remains at 7.5. The mixture was then admixed with water (30 ml) and filtered through kieselguhr and washed several more times with water. The aqueous phase was then extracted with dichloromethane (3×30 ml), and the organic phase was dried (Na2SO4) and concentrated. This gave the product (1.3 g) with an ee=90% by HPLC.
後処理
- additionAfter addition of Amano Lipase PS (150 mg)
- filtrationfiltered through kieselguhr
- washwashed several more times with water
- extractionThe aqueous phase was then extracted with dichloromethane (3×30 ml)
- dry with materialthe organic phase was dried (Na2SO4)
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-50215cbfa0844d518cd67d540ea07104
- 出典データセット
- uspto-grants-2014_11
- 特許番号
- US08895547B2
反応ノート
読み込み中…