HRID1082126
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
- 80 °C
PROCEDURE
实验过程
A mixture of methyl 3-(4-benzyloxyphenyl)-2-chloropropanoate (International Patent Appl., Publication No. WO 9101337) (0.50 g), sodium benzenesulphinate (0.29 g) and dry N,N-dimethylformamide (25 mL) was heated at 80° C. for 24 hrs. The mixture was cooled and diluted with water (500 mL), then extracted with dichloromethane (2×250 mL). The combined organic solutions were washed with water (2×250 mL) and brine (250 mL), dried (MgSO4) and evaporated. The residue was chromatographed on silica gel with dichloromethane as eluent to afford the title compound.
WORKUP
后处理
- temperatureThe mixture was cooled
- extractionextracted with dichloromethane (2×250 mL)
- washThe combined organic solutions were washed with water (2×250 mL) and brine (250 mL)
- dry with materialdried (MgSO4)
- customevaporated
- customThe residue was chromatographed on silica gel with dichloromethane as eluent