HRID453092
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
- 150 °C
PROCEDURE
实验过程
To a solution of 5-(4-methoxyphenyl)-[1,3,4]oxathiazol-2-one (0.47 g, 2.24 mmol) in n-dodecane (0.70 ml) was added ethyl cyanoformate (0.90 ml, 8.10 mmol). The resulting reaction mixture was refluxed for 20 h at 150° C. After the completion of the reaction (TLC monitoring), added ice-cold water and extracted with ethyl acetate (3×50 ml). The combined organic layer was dried over Na2SO4, filtered and concentrated under vacuum. The crude residue washed with ether to get the desired product (0.24 g, 40%). MS ES+ (265.08).
WORKUP
后处理
- customThe resulting reaction mixture
- customAfter the completion of the reaction (TLC monitoring)
- additionadded ice-cold water
- extractionextracted with ethyl acetate (3×50 ml)
- dry with materialThe combined organic layer was dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated under vacuum
- washThe crude residue washed with ether