反应详情

A solution of 3-trifluoroacetyl-2,3,4,5-tetrahydro-1H-3-benzazepine (see WO02/40471) (20 g, 80 mmol) in dichloromethane (50 mL) was added dropwise to a solution of chlorosulfonic acid (33 mL, 240 mmol) in more dichloromethane (200 mL) at 0° C. The resulting solution was stirred for 18 h without cooling then poured onto ice (250 g). The resulting organic layer was washed with brine (100 mL), dried (MgSO4), and evaporated to give the subtitle compound as a white solid (23 g).

1. temperaturewithout cooling
2. additionthen poured onto ice (250 g)
3. washThe resulting organic layer was washed with brine (100 mL)
4. dry with materialdried (MgSO4)
5. customevaporated