HRID355622

反应详情

EQUATION

反应方程式

HRID 355622 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

5.68 pbw of 2-amino-9-(4-methylphenyl)acridine (compound 12d) were dissolved with 20.3 pbw of methanesulfonyl chloride and 22.4 pbw of diazabicyclo[2.2.2]octane in 120 pbv of acetonitrile and the solution heated for 2 hours under reflux. After cooling to 20° C., filtration was carried out and the red filtrate added dropwise to 1000 pbv of 0.5% strength ammonia solution. After standing overnight, the precipitate was filtered off by suction and crystallized from 135 pbv of ethanol. Yield: 1.76 pbw (20% of theory), light yellow needles. Mp.: 217°-219° C.

WORKUP

后处理

  1. temperaturethe solution heated for 2 hours
  2. temperatureunder reflux
  3. filtrationfiltration
  4. additionthe red filtrate added dropwise to 1000 pbv of 0.5% strength ammonia solution
  5. filtrationthe precipitate was filtered off by suction
  6. customcrystallized from 135 pbv of ethanol