HRID2203077
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
To a suspension of 1-(2-cyclopropyl-1-methyl-1H-benzimidazol-6-yl)-4-hydroxypyridin-2(1H)-one (2 g) in DMF (35 ml) was added phosphoryltribromide (2.45 g) at room temperature, and the mixture was stirred at 50° C. overnight. The mixture was poured into saturated NaHCO3 solution, and extracted with EtOAc. The organic layer was washed with water and brine successively, dried over MgSO4 and concentrated in vacua. The resulting residual solid was recrystallized from EtOH-hexane to give the title compound (1.70 g) as a brown solid.
WORKUP
后处理
- extractionextracted with EtOAc
- washThe organic layer was washed with water and brine successively
- dry with materialdried over MgSO4
- concentrationconcentrated in vacua
- customThe resulting residual solid was recrystallized from EtOH-hexane