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
- 50 °C
PROCEDURE
实验过程
A solution of (RS) ethyl 3-{5-[2-(3-acetoxy-4-nitrophenyl)-acetylamino]-pyridin-2-yl}-butanoate (6.18 g, Reference Example 27) in methanol (100 mL) was treated with a solution of sodium hydroxide (3.5 g) in water (20 mL). The mixture was heated at 50° C. for 5 hours and then evaporated. The residue was dissolved in water and the resulting solution was washed with ethyl acetate, then acidified to pH 5 by addition of glacial acetic acid and then extracted with ethyl acetate. The extracts were washed with water, then dried over magnesium sulphate and then evaporated. The residual dark oil was subjected to flash chromatography on silica eluting with ethyl acetate to give the title compound (2.1 g) as a brown solid.
WORKUP
后处理
- customevaporated
- dissolutionThe residue was dissolved in water
- washthe resulting solution was washed with ethyl acetate
- additionacidified to pH 5 by addition of glacial acetic acid
- extractionextracted with ethyl acetate
- washThe extracts were washed with water
- dry with materialdried over magnesium sulphate
- customevaporated