反応式
C(N(S(F)(F)F)CC)C.[Cl:10][C:11]1[CH:12]=[CH:13][C:14]([C:41]#[N:42])=[C:15]([C:17]2[C:22]([O:23][CH3:24])=[CH:21][N:20]([CH:25]([CH:33](O)[CH:34]3[CH2:38][CH2:37][O:36][CH2:35]3)[C:26]([O:28][C:29]([CH3:32])([CH3:31])[CH3:30])=[O:27])[C:19](=[O:40])[CH:18]=2)[CH:16]=1.C(=O)(O)[O-].[Na+]>ClCCl>[Cl:10][C:11]1[CH:12]=[CH:13][C:14]([C:41]#[N:42])=[C:15]([C:17]2[C:22]([O:23][CH3:24])=[CH:21][N:20]([C:25](=[CH:33][CH:34]3[CH2:38][CH2:37][O:36][CH2:35]3)[C:26]([O:28][C:29]([CH3:31])([CH3:30])[CH3:32])=[O:27])[C:19](=[O:40])[CH:18]=2)[CH:16]=1参加物
5
反応物 3
生成物 1
試薬・触媒・溶媒 1
実験手順
At RT, 0.5 ml (3.8 mmol, 1.2 eq.) of diethylaminosulphur trifluoride was added dropwise to a solution of 1.55 mg (3.13 mmol) of tert-butyl 2-[4-(5-chloro-2-cyanophenyl)-5-methoxy-2-oxopyridin-1(2H)-yl]-3-hydroxy-3-(tetrahydrofuran-3-yl)propanoate (diastereomer mixture) in 48 ml of dichloromethane, the mixture was stirred at RT for 90 min and 50 ml of dichloromethane and 50 ml of saturated aqueous sodium bicarbonate solution were then added. After phase separation, the aqueous phase was extracted with dichloromethane. The combined organic phases were washed with saturated aqueous sodium chloride solution, dried (sodium sulphate), filtered, concentrated under reduced pressure and dried. Yield: 1.38 g (93% of theory)
後処理
- customAfter phase separation
- extractionthe aqueous phase was extracted with dichloromethane
- washThe combined organic phases were washed with saturated aqueous sodium chloride solution
- dry with materialdried (sodium sulphate)
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customdried
出典と根拠
- ORDレコード
- ord-52fe372853a54386b7cb428a3a08a36e
- 出典データセット
- uspto-grants-2016_09
- 特許番号
- US09434690B2
関連ノート
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