HRID1698541

反应详情

EQUATION

反应方程式

HRID 1698541 的结构方程式

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

7-Bromo-1-methyl-1,3-dihydro-2H-benzimidazol-2-one (2.20 g, 9.69 mmol) was dissolved in 30 mL of phosphorous oxychloride and the mixture was heated at 110° C. for 2 days. The reaction allowed to cool to room temperature, poured into water with an ice, and stirred for 1 h. The aqueous solution was extracted with ethyl acetate. The extract was washed with aqueous sodium bicarbonate, dried over magnesium sulfate, filtered and concentrated in vacuo to give 2.32 g of the title compound, which was used in the next reaction without further purification.

WORKUP

后处理

  1. temperatureto cool to room temperature
  2. extractionThe aqueous solution was extracted with ethyl acetate
  3. washThe extract was washed with aqueous sodium bicarbonate
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo