HRID1736356
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
The crude ester (10 g, 38 mM) was dissolved in ethanol (20 ml) and added to a stirred suspension of SnCl2.2H2O (42.9 g, 0.19M) in ethanol (60 ml) under argon at ambient temperature. The mixture was heated to reflux for 30 minutes, cooled and poured onto ice. After making basic to pH 8 with an aqueous solution of sodium bicarbonate, the mixture was extracted with ethyl acetate. The combined extracts were washed with water and brine, dried over MgSO4 and evaporated to give allyl 3-allyloxy-4-aminobenzoate (8.2 g).
WORKUP
后处理
- temperatureThe mixture was heated
- temperatureto reflux for 30 minutes
- temperaturecooled
- additionpoured onto ice
- extractionthe mixture was extracted with ethyl acetate
- washThe combined extracts were washed with water and brine
- dry with materialdried over MgSO4
- customevaporated