反应详情

Sodium, 3.0 g. (0.13 mole), was added piecewise under a nitrogen atmosphere to 100 ml. of dry methanol, followed by the addition of a slurry of 31.6 g. (0.1 mole) of 5,6-bis(4-methoxyphenyl)-3-methylthio-1,2,4-triazine in methanol. The reaction mixture was heated at reflux overnight. The reaction mixture was cooled and filtered. The filter cake and filtrate were extracted with diethyl ether. The diethyl ether was concentrated, giving a solid, m.p. >220° C. The solid was taken up in diethyl ether and the insoluble material was removed by filtration. The filtrate was dried over anhydrous sodium sulfate and concentrated to give a solid residue which was recrystallized from petroleum ether to give 3-methoxy-5,6-bis(4-methoxyphenyl)-1,2,4-triazine, m.p. about 105°-108° C.

1. addition(0.13 mole), was added piecewise under a nitrogen atmosphere to 100 ml
2. temperatureThe reaction mixture was heated
3. temperatureat reflux overnight
4. temperatureThe reaction mixture was cooled
5. filtrationfiltered
6. extractionThe filter cake and filtrate were extracted with diethyl ether
7. concentrationThe diethyl ether was concentrated
8. customgiving a solid, m.p. >220° C
9. customthe insoluble material was removed by filtration
10. dry with materialThe filtrate was dried over anhydrous sodium sulfate
11. concentrationconcentrated
12. customto give a solid residue which
13. customwas recrystallized from petroleum ether