HRID384738

反应详情

EQUATION

反应方程式

HRID 384738 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Nelfinavir base (15 g) is suspended in methanol (22.5 ml), and methanesulfonic acid (2.55 g) is added at temperature below 45° C. over 30 min. The reaction mixture is maintained at 40° C. to 45° C. for 1 hr to get clear solution. The obtained clear solution is cooled to a temperature of 25° C. to 30° C., acetone (87 ml) is added over 30 min and mixed for 2 hrs at 25° C. to 30° C. The reaction mass is cooled to 0° C. to 5° C. and maintained for 2 hrs. The precipitated solid is filtered, washed with chilled acetone (7.5 ml) and dried at 90° C. to 100° C. under vacuum till becomes constant weight.

WORKUP

后处理

  1. temperatureThe reaction mixture is maintained at 40° C. to 45° C. for 1 hr
  2. customto get clear solution
  3. additionis added over 30 min
  4. additionmixed for 2 hrs at 25° C. to 30° C
  5. temperatureThe reaction mass is cooled to 0° C. to 5° C.
  6. temperaturemaintained for 2 hrs
  7. filtrationThe precipitated solid is filtered
  8. washwashed with chilled acetone (7.5 ml)
  9. customdried at 90° C. to 100° C. under vacuum