HRID468600
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
To a stirred solution of ester 9 (2.66 g, 10 mmol) in dichloromethane (91 ml) was added TFA (9 ml) reaction mixture was stirred at room temperature for 2 hrs and mixture was concentrated. Obtained residue was diluted in water and basified with a NaOH 1N solution. This aqueous layer was extracted with ether then acidified and extracted twice with EtOAc. Combined organic layers were dried over MgSO4, filtered and concentrated to give acid 10 (2 g, 95%) as an oil, used for next step without further purification.
WORKUP
后处理
- concentrationmixture was concentrated
- additionObtained residue was diluted in water
- extractionThis aqueous layer was extracted with ether
- extractionextracted twice with EtOAc
- dry with materialCombined organic layers were dried over MgSO4
- filtrationfiltered
- concentrationconcentrated