HRID132690
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of compound 2A (6.20 g, 26.7 mmol) in MeOH (100 mL) was treated with saturated aqueous LiOH (15 mL), and the reaction mixture was stirred at rt overnight (˜16 h). The resulting mixture was concentrated in vacuo to dryness and partitioned between a mixed solvent (50% Et2O:50% EtOAc) and H2O. The H2O layer was acidified to pH 2-3 and extracted with EtOAc (3×20 mL). The EtOAc was dried over Na2SO4 and concentrated in vacuo to give a yellow solid (2.1 g) in 38% yield.
WORKUP
后处理
- concentrationThe resulting mixture was concentrated in vacuo to dryness
- custompartitioned between a mixed solvent (50% Et2O:50% EtOAc) and H2O
- extractionextracted with EtOAc (3×20 mL)
- dry with materialThe EtOAc was dried over Na2SO4
- concentrationconcentrated in vacuo