HRID2361508

反应详情

EQUATION

反应方程式

HRID 2361508 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

Phosphorus oxybromide (25 g, 87 mmol) was added to a suspension of benzo[4,5]imidazo[1,2-a]pyrimidin-2-ol (5.2 g, 28.1 mmol) in DCE (Ratio: 1.000, Volume: 93 ml) and DMF (Ratio: 0.01, Volume: 0.927 ml). Heated the reaction mixture to 100° C. for 3 hours. Cooled the reaction to room temperature and concentrated. Diluted with ice water and quenched to pH ˜8 with concentrated ammonium hydroxide. The resulting residue was filtered and washed with water followed by ethyl ether. Dried under vacuum to afford crude 2-bromobenzo[4,5]imidazo[1,2-a]pyrimidine (6.97 g, 28.1 mmol, 100% yield).

WORKUP

后处理

  1. temperatureCooled
  2. customthe reaction to room temperature
  3. concentrationconcentrated
  4. additionDiluted with ice water
  5. customquenched to pH ˜8 with concentrated ammonium hydroxide
  6. filtrationThe resulting residue was filtered
  7. washwashed with water
  8. customDried under vacuum