反応式
[Si:1]([O:8][C:9]1([CH2:12][CH:13]=O)[CH2:11][CH2:10]1)([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2].[Si](O)(CC)(CC)CC.[CH3:23][C:24]([S@:27]([NH2:29])=[O:28])([CH3:26])[CH3:25]>C(Cl)Cl>[Si:1]([O:8][C:9]1([CH2:12]/[CH:13]=[N:29]/[S@@:27]([C:24]([CH3:26])([CH3:25])[CH3:23])=[O:28])[CH2:11][CH2:10]1)([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2]参加物
5
反応条件
- 温度
- 23 °C
実験手順
To a 1.0 L round bottom flask containing 2-(1-(tert-butyldimethylsilyloxy)cyclopropyl)acetaldehyde (5.00 g, 23.3 mmol) (crude 10.5 g with TESOH, 1H NMR showed about 50/50 sm to impurity) was added DCM (200 mL) and the mixture was allowed to stir at 23° C. for 5 min. At this time, (R)-2-methylpropane-2-sulfinamide (2.83 g, 23.3 mmol) and cupric sulfate anhydrous (2.58 ml, 58.3 mmol) were added and the reaction was allowed to stir for 40 h. The copper salts were removed by celite filtration. The filtrate was concentrated to give a yellow oil that was purified on a 330 g Isco column (5 to 20% EtOAc in hexanes)to afford the title compound as a colorless oil.
後処理
- stirringto stir for 40 h
- customThe copper salts were removed by celite filtration
- concentrationThe filtrate was concentrated
- customto give a yellow oil that
- customwas purified on a 330 g Isco column (5 to 20% EtOAc in hexanes)
出典と根拠
- ORDレコード
- ord-97b820d84b6847df95d2262091e04ca6
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07745484B2
関連ノート
読み込み中…