反应详情

A stirred suspension of (cis)-3-(hydroxy)-1-[2-(dimethylamino)ethyl]-1,3,4,5-tetrahydro-4-(4-methoxyphenyl)-7-(trifluoromethyl)-2H-1-benzazepin-2-one, monohydrochloride (1.50 g; 3.27 mmol) in 50 ml of acetic anhydride was heated in an oil bath at 110°-117° C. (solution obtained) for 2.5 hours (under argon). TLC (8:1:1 dichloromethane-methanol-acetic acid) showed the reaction to be complete. The acetic anhydride was removed on a rotary evaporator at 0.2 mm to give a solid. The latter was rubbed under ethyl acetate, 1 ml of saturated hydrogen chloride in ether (to pH 2) was added and the evaporation repeated. The colorless material was rubbed under ether, cooled overnight, filtered, washed in ether, and dried in vacuo; yield 1.43 g; melting point 230°-232° C. (dec.); s. 227° C. TLC: Rf =0.41 (8:1:1 dichloromethane-methanol-acetic acid).

1. temperaturewas heated in an oil bath at 110°-117° C.
2. custom(solution obtained) for 2.5 hours (under argon)
3. customthe reaction
4. customThe acetic anhydride was removed on a rotary evaporator at 0.2 mm
5. customto give a solid
6. customthe evaporation
7. temperaturecooled overnight
8. filtrationfiltered
9. washwashed in ether
10. customdried in vacuo
11. custom227° C