反应详情

1-(2-chlorophenyl)-5(4H)-tetrazolinone (2 g) and potassium carbonate (1.68 g) were suspended in acetonitrile (30 ml), followed by fifteen minutes heating under refluxing. After cooling, N-cyclohexyl-N-ethylcarbamoyl chloride (2.31 g) was added to the reaction mixture, followed by a further five-hour heating under refluxing. The resulting mixture was filtered and the filtrate was evaporated under reduced pressure, and the resulting residue was subjected to flush column chromatography (hexane:ethylacetate=5:2), to obtain the desired 1-(2-chlorophenyl)-4-(N-cyclohexyl-N-ethylcarbamoyl)- 5(4H)-tetrazolinone (3.02 g) having a m.p. in the range of from 77.5° to 79.5° C.

1. waitfollowed by fifteen minutes
2. temperatureheating
3. temperatureunder refluxing
4. temperatureAfter cooling
5. waitfollowed by a further five-hour
6. temperatureheating
7. temperatureunder refluxing
8. filtrationThe resulting mixture was filtered
9. customthe filtrate was evaporated under reduced pressure
10. customto flush column chromatography (hexane:ethylacetate=5:2)