反応 #44486

反応方程式

solution

4-(tert-Butyl-dimethyl-silanyloxymethyl)-1-cycloheptyl-3,3-dimethyl-pyrrolidin-2-one

Dess-Martin periodinane

→

title compound

1-Cycloheptyl-4,4-dimethyl-5-oxo-pyrrolidine-3-carbaldehyde

溶媒

methanol

反応条件

後処理

1. 1
   その他The solvent was evaporated in vacuo
2. 2
   workup.STIRRINGstirred at room temperature for two hours
3. 3
   その他The reaction was quenched with 10% sodium bisulfite
4. 4
   抽出extracted with dichloromethane
5. 5
   洗浄The organic phase was washed with water
6. 6
   乾燥dried with MgSO4
7. 7
   ろ過filtered
8. 8
   その他evaporated in vacuo

実験手順

To a solution of Example 1D (0.168 mg, 0.475 mmoles) in methanol (1.5 mL), two drops of 12M HCl was added and stirred for one hour. The solvent was evaporated in vacuo. The residue was taken in dichloromethane (2.5 mL) and Dess-Martin periodinane (0.25 gm, 0.593 mmoles) was added and stirred at room temperature for two hours. The reaction was quenched with 10% sodium bisulfite and extracted with dichloromethane. The organic phase was washed with water, dried with MgSO4, filtered, and evaporated in vacuo to provide the title compound.

出典