HRID254874

反应详情

EQUATION

反应方程式

HRID 254874 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 4-(oxiran-2-ylmethoxy)-9H-carbazole (II) (25.0 g, 104.60 mmole) and 62.5 ml 2-propanol is heated to 70° C. to 80° C. To this 2-(2-methoxyphenoxy)ethylamine (III) (25.33 g, 151.67 mmole) is added in one lot. The temperature of reaction mass is raised to reflux (80° C. to 85° C.) and maintain at this reaction temperature for one hour. After that, this reaction mass is added to the pre-heated (80° C. to 85° C.) solution of oxalic acid (14.6 g) (162.13 mmole) in 2-propanol (287.5 ml) and continued the reflux for next one-hour, cooled to 50° C. to 55° C. and maintain for 1 hour. The product is filtered at the same temperature followed by three 33.5 ml wash with hot (50° C. to 55° C.) 2-propanol. The wet product dried at 60° C. to 65° C. for 6-8 hours or till constant weight gives 42.0 g of Carvedilol Oxalate (Yield 80.95%).

WORKUP

后处理

  1. temperatureis heated to 70° C. to 80° C
  2. customThe temperature of reaction mass
  3. temperatureis raised
  4. temperatureto reflux (80° C. to 85° C.)
  5. temperaturemaintain at this reaction temperature for one hour
  6. additionAfter that, this reaction mass is added to the
  7. temperaturereflux for next one-hour
  8. temperaturecooled to 50° C. to 55° C.
  9. temperaturemaintain for 1 hour
  10. filtrationThe product is filtered at the same temperature
  11. washwash with hot (50° C. to 55° C.) 2-propanol
  12. customThe wet product dried at 60° C. to 65° C. for 6-8 hours or till constant weight