HRID1184970
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 solution of 4-(formyloxy)-2-methoxyphenyl acetate (16 g, 76 mmol) in THF (50 mL)/H2O (50 mL) was added LiOH (7.7 g, 184.2 mmol). The reaction was stirred at room temperature overnight. The volatiles were removed under reduced pressure. The residue was extracted with EA (50 mL×3). The organic phase was washed with brine (50 mL), dried over Na2SO4, filtrated and concentrated in vacuo to give black oil, which was purified by silica gel column (PE:EA=3:1) to afford 4.8 g of product (40%) as a brown solid.
WORKUP
后处理
- customThe volatiles were removed under reduced pressure
- extractionThe residue was extracted with EA (50 mL×3)
- washThe organic phase was washed with brine (50 mL)
- dry with materialdried over Na2SO4
- filtrationfiltrated
- concentrationconcentrated in vacuo
- customto give black oil, which
- customwas purified by silica gel column (PE:EA=3:1)