HRID1465803
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
CONDITIONS
反应条件
- 温度
- 62.5 °C
PROCEDURE
实验过程
To a solution of methyl 4-amino-2-methoxybenzoate (501 mg, 2.77 mmol) in ethanol (8 ml) was added acetic anhydride (0.42 ml, 4.44 mmol, 1.6 eq) and the clear solution heated at 60-65° C. for 2 h. After cooling to room temperature the solvent was removed by rotary evaporator and the residue treated with water (10 ml) and saturated sodium bicarbonate solution (10 ml) before extracting with ethyl acetate (20 ml, 2×10 ml). The combined ethyl acetate extract was washed with water, then brine, dried (MgSO4) and evaporated to give methyl 4-acetamido-2-methoxybenzoate (545 mg, 88%) as a white solid.
WORKUP
后处理
- temperatureAfter cooling to room temperature the solvent
- customwas removed by rotary evaporator
- additionthe residue treated with water (10 ml) and saturated sodium bicarbonate solution (10 ml)
- extractionbefore extracting with ethyl acetate (20 ml, 2×10 ml)
- extractionThe combined ethyl acetate extract
- washwas washed with water
- dry with materialbrine, dried (MgSO4)
- customevaporated