反应详情

温度

60 °C

A mixture of 1-(3-bromopropyl)-3-methyl-2,4(1H, 3H)-quinazolinedione (1.68 g), 1-diphenylmethylpiperazine (1.56 g), anhydrous potassium carbonate (2.33 g) and N,N-dimethylformamide (8 ml) was stirred for 3 hours at 60° C. After cooling, water was added to the reaction mixture and then the mixture was extracted twice with chloroform. The chloroform layer was washed with water and with saturated sodium chloride aqueous solution respectively, dried over anhydrous magnesium sulfate and evaporated in vacuo to give an oily residue. This oily residue was dissolved in methanol and then conc.hydrochloric acid solution was dropwise added to the solution to give a crystal, which was collected by filtration, washed with water and dried. This crude crystal was recrystallized from a mixture of methanol and water to give 1-[3-{4-(diphenylmethyl)-piperazin-1-yl}propyl]-3-methyl-2,4(1H, 3H)-quinazolinedione.2HCl.0.5H20 (2.4 g). m.p. 250°-253° C.

1. temperatureAfter cooling
2. extractionthe mixture was extracted twice with chloroform
3. washThe chloroform layer was washed with water and with saturated sodium chloride aqueous solution respectively
4. dry with materialdried over anhydrous magnesium sulfate
5. customevaporated in vacuo
6. customto give an oily residue
7. customto give a crystal, which
8. filtrationwas collected by filtration
9. washwashed with water
10. customdried
11. customThis crude crystal was recrystallized from a mixture of methanol and water