反应详情

A solution of 1.0 g of 3-fluoro-10-[4-(2-hydroxyethyl)piperazino]-8-isopropyl-10,11-dihydrodibenzo(b,f)thiepin base (Example 3) in 5 ml chloroform was treated with 0.5 g acetic anhydride and the mixture allowed to stand overnight at room temperature. It was then diluted with 20 ml of chloroform, washed with water and with ice-cold sodium hydroxide solution, dried with potassium carbonate, and the chloroform evaporated under reduced pressure. The remaining oil (1.1 g, 100%) was dissolved in 3.5 ml of acetone and the solution neutralized under heating with 0.6 g maleic acid. On cooling, 1.3 g (77%) of dimaleate crystallized which was then recrystallized from acetone and melted at 153°-155.5° C.; it was identical with the product obtained by a different way according to Example 14.

1. washwashed with water and with ice-cold sodium hydroxide solution
2. dry with materialdried with potassium carbonate
3. customthe chloroform evaporated under reduced pressure
4. dissolutionThe remaining oil (1.1 g, 100%) was dissolved in 3.5 ml of acetone
5. temperatureunder heating with 0.6 g maleic acid
6. temperatureOn cooling
7. custom1.3 g (77%) of dimaleate crystallized which
8. customwas then recrystallized from acetone and melted at 153°-155.5° C.
9. customobtained by a different way