反应详情

At ~25°, a solution of 2-chloro-4-(1-piperaziny)-benzenemethanol 3.0 g, 13.2 mmole) in 30 ml of tetrahydrofuran and 4 ml of triethylamine was added during five minutes to a solution of 3-chloro-1-(2-furanyl)-1-propanone (2.8 g. 13.3 mmole based on 75% purity). The mixture was stirred at 25° for one hour (a white precipitate formed) and was then heated under reflux for one half hour. The mixture was then filtered and the filtrate was evaporated at reduced pressure (<40°) to give an orange, heavy oil. The oil was triturated at 25° first with petroleum ether (30°-60°; two times, 50 ml) and then with diethyl ether. The orange-brown solid was collected, washed with a little diethyl ether, recrystallized from 25 ml of toluene, and finally triturated with diethyl ether (two times, 20 ml) and dried to give 3.10 g (67%), mp 95°-98° (Table 3).

1. customformed) and
2. temperaturewas then heated
3. temperatureunder reflux for one half hour
4. filtrationThe mixture was then filtered
5. customthe filtrate was evaporated at reduced pressure (<40°)
6. customto give an orange, heavy oil
7. customThe oil was triturated at 25° first with petroleum ether (30°-60°; two times, 50 ml)
8. customThe orange-brown solid was collected
9. washwashed with a little diethyl ether
10. customrecrystallized from 25 ml of toluene
11. customfinally triturated with diethyl ether (two times, 20 ml)
12. customdried
13. customto give 3.10 g (67%), mp 95°-98° (Table 3)