HRID2203077

反应详情

EQUATION

反应方程式

HRID 2203077 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. extractionextracted with EtOAc
  2. washThe organic layer was washed with water and brine successively
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated in vacua
  5. customThe resulting residual solid was recrystallized from EtOH-hexane