HRID384738
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThe reaction mixture is maintained at 40° C. to 45° C. for 1 hr
- customto get clear solution
- additionis added over 30 min
- additionmixed for 2 hrs at 25° C. to 30° C
- temperatureThe reaction mass is cooled to 0° C. to 5° C.
- temperaturemaintained for 2 hrs
- filtrationThe precipitated solid is filtered
- washwashed with chilled acetone (7.5 ml)
- customdried at 90° C. to 100° C. under vacuum