反应详情

温度

17.5 °C

Methanol (1200 ml) and 6-(3-morpholino propoxy)-7-methoxy-4-chloro quinazoline (200 gm) were stirred for 15 minutes at 25-30° C., then a solution of 4-fluoro-3-chloroaniline in methanol (213 gm in 400 ml) was charged and refluxed for 6 hours. The reaction mass was cooled to 15-20° C., hydrochloric acid (40 ml) was added drop wise, and stirred at 5-10° C. for 30 minutes. The solid obtained was filtered and washed with chilled methanol (150 ml). The solid was dissolved in a mixture of toluene (30 volume) and methanol (5 volume), the reaction mass was concentrated to half the volume and cooled to 5-10° C. The solid obtained was filtered, washed with toluene (200 ml) and dried at 45-50° C. to yield the title compound (183 gm, 70% yield).

1. temperaturerefluxed for 6 hours
2. customThe solid obtained
3. filtrationwas filtered
4. washwashed with chilled methanol (150 ml)
5. dissolutionThe solid was dissolved in a mixture of toluene (30 volume) and methanol (5 volume)
6. concentrationthe reaction mass was concentrated to half the volume
7. temperaturecooled to 5-10° C
8. customThe solid obtained
9. filtrationwas filtered
10. washwashed with toluene (200 ml)
11. customdried at 45-50° C.