反应详情

0.6 g of sodium hydride (60% oily dispersion) is added to a solution of 3.0 g of phenothiazine in 20 ml of anhydrous dimethylformamide under argon, then the reaction mixture is stirred at 50° to 60° C. for 2 hours. Thereafter, 3.9 g of 8-(3-chloropropyl)-3-ethyl-4-methylene-2-oxo-1-oxa-3,8-diazaspiro[4,5]decane dissolved in 20 ml of dimethylformamide are dropwise added and the mixture is stirred at 40° to 50° C. for additional 6 to 7 hours. After cooling down saturated ammonium chloride solution is added to the reaction mixture under argon and the solvent is evaporated under reduced pressure. After taking up the evaporation residue in benzene and washing the benzene solution with water the solution is dried over anhydrous sodium sulfate and then evaporated under reduced pressure. The residue is recrystallized from ethanol to give the title product in 57.6% yield, m.p.: 122°-123° C.

1. additionare dropwise added
2. stirringthe mixture is stirred at 40° to 50° C. for additional 6 to 7 hours
3. additionis added to the reaction mixture under argon
4. customthe solvent is evaporated under reduced pressure
5. washwashing the benzene solution with water the solution
6. dry with materialis dried over anhydrous sodium sulfate
7. customevaporated under reduced pressure
8. customThe residue is recrystallized from ethanol