反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
3-(1-tert-butyl-5-(4-chlorophenyl)-1H-pyrazol-3-yl)propan-1-ol (200 mg, 0.774 mmol), PCC (334 mg, 1.548 mmol), SiO2 (334 mg) was added with 5 mL of CH2Cl2 under nitrogen atmosphere and stirred for 5 hrs at room temperature. The progress and completion of the reaction were confirmed by means of TLC. Upon completion of the reaction, the reaction mixture was cooled down to room temperature and the solvent was removed from the reaction mixture under reduced pressure. The reaction mixture was diluted with EtOAc, and added with water. The aqueous layer was extracted with EtOAc and the organic layer was dried with anhydrous MgSO4 and filtered. The resulting filtrate was concentrated under reduced pressure and the resulting concentrate was passed through column chromatography (Ether:Hexane=2:3, v/v) to obtain 149 mg (75%) of target compound.
WORKUP
后处理
- customUpon completion of the reaction
- temperaturethe reaction mixture was cooled down to room temperature
- customthe solvent was removed from the reaction mixture under reduced pressure
- additionThe reaction mixture was diluted with EtOAc
- additionadded with water
- extractionThe aqueous layer was extracted with EtOAc
- dry with materialthe organic layer was dried with anhydrous MgSO4
- filtrationfiltered
- concentrationThe resulting filtrate was concentrated under reduced pressure
- concentrationthe resulting concentrate
- customHexane=2:3, v/v) to obtain 149 mg (75%) of target compound