HRID453107
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
- 120 °C
PROCEDURE
实验过程
To a solution of [3-(4-benzyloxyphenyl)-[1,2,4]thiadiazol-5-yl]-methanol (0.052 g, 0.17 mmol) in toluene (5 ml) was added PBr3 (0.027 ml, 0.26 mmol) and the resulting reaction mixture was refluxed at 120° C. for 15 min. After the completion of the reaction (TLC monitoring), the reaction mixture was cooled to 0° C., added water (50 ml) and extracted with ethyl acetate (3×50 ml). The combined organics was washed with saturated NaHCO3 solution, dried over Na2SO4, filtered and concentrated under vacuum to get the desired product (0.043 g, 68%).
WORKUP
后处理
- customthe resulting reaction mixture
- customAfter the completion of the reaction (TLC monitoring)
- temperaturethe reaction mixture was cooled to 0° C.
- extractionextracted with ethyl acetate (3×50 ml)
- washThe combined organics was washed with saturated NaHCO3 solution
- dry with materialdried over Na2SO4
- filtrationfiltered
- concentrationconcentrated under vacuum