反应详情

To 80 ml of toluene were added 8.0 g (40 m moles) of 1-(4,6-dimethoxypyrimidine-2-yl)-2-propanone and 7.9 g (44 m moles) of 4-chlorophenylhydrazine hydrochloride. Thereto was added 6.54 g (48 m moles) of zinc chloride. Refluxing was made for 2 hours with heating. The reaction mixture was allowed to cool. Then, ethyl acetate and water were added to dissolve the whole reaction mixture. The organic layer was washed with water, separated, and dried over Glauber's salt. The resulting organic layer was concentrated under reduced pressure using a rotary evaporator to obtain an orange solid. The solid was washed with isopropyl ether to obtain 10.2 g (33.7 m moles) of 5-chloro-3-(4,6-dimethoxypyrimidine-2-yl)-2-methylindole. Yield: 84% Melting point: 179 to 181° C.

1. temperatureRefluxing
2. temperaturewith heating
3. temperatureto cool
4. dissolutionto dissolve
5. customthe whole reaction mixture
6. washThe organic layer was washed with water
7. customseparated
8. dry with materialdried over Glauber's salt
9. concentrationThe resulting organic layer was concentrated under reduced pressure
10. customa rotary evaporator
11. customto obtain an orange solid
12. washThe solid was washed with isopropyl ether