反应详情

温度

2.5 °C

To a suspension of (R)-5-(2-(benzylamino)ethyl)-1-(6,8-difluorochroman-3-yl)-1H-imidazole-2(3H)-thione (2 g, 4.98 mmol) in methanol (MeOH) (30 ml) was added 1.5M hydrochloric acid (3.32 ml, 4.98 mmol) in MeOH to give a clear solution. To the solution Toluene (30.0 ml) was added, MeOH (30 ml) was removed on a rotavap followed by addition of toluene (20 ml). The mixture was aged with stirring for 1 hours at 0-5° C., the precipitate collected, washed with toluene (10 ml), dried in vacuum at 50° C. to give 2.05 g (94%) of purified (R)-5-(2-(benzylamino)ethyl)-1-(6,8-difluorochroman-3-yl)-1H-imidazole-2(3H)-thione hydrochloride.

1. customto give a clear solution
2. customMeOH (30 ml) was removed on a rotavap
3. additionfollowed by addition of toluene (20 ml)
4. customthe precipitate collected
5. washwashed with toluene (10 ml)
6. customdried in vacuum at 50° C.