反应详情

Nelfinavir base (25 g) is suspended in THF (75 ml), and methanesulfonic acid (4.25 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 28° C. to 30° C. and methyl ethyl ketone (145 ml) is added over 20 min, mixed at temperature of 25° C. to 30° C. for 2 hrs. The reaction mass is cooled and maintained at 0° C. to 5° C. for 2 hrs. The precipitated solid is filtered, washed with chilled methyl ethyl ketone (12.5 ml) and dried at 90° C. to 100° C. under vacuum till becomes constant weight.

1. temperatureThe reaction mixture is maintained at 40° C. to 45° C. for 1 hr
2. customto get clear solution
3. temperatureThe obtained clear solution is cooled to 28° C. to 30° C.
4. additionmixed at temperature of 25° C. to 30° C. for 2 hrs
5. temperatureThe reaction mass is cooled
6. temperaturemaintained at 0° C. to 5° C. for 2 hrs
7. filtrationThe precipitated solid is filtered
8. washwashed with chilled methyl ethyl ketone (12.5 ml)
9. customdried at 90° C. to 100° C. under vacuum