반응 #926763

반응 방정식

2-imidazolecarboxylic acid hydrazide

trimethylorthobenzoate

→

desired product

5-phenyl-imidazo[1,2-d]-as-triazin-8(7H)-one

용매

ethanol

반응 조건

후처리

1. 1
   workup.ADDITIONTo this is added 20 ml
2. 2
   온도The mixture is refluxed for 31 hours
3. 3
   기타the solvents are evaporated
4. 4
   기타giving a white solid which
5. 5
   세척is washed twice with diethyl ether giving 3.0 gm
6. 6
   온도of diphenyl ether and heated
7. 7
   온도The mixture is cooled
8. 8
   workup.ADDITIONpetroleum ether is added
9. 9
   여과the mixture is filtered
10. 10
    세척The solid is washed twice with hot petroleum ether
11. 11
    기타giving 1.4 gm

실험 절차

A 2.6 gm. portion of 2-imidazolecarboxylic acid hydrazide is added to 200 ml. of ethanol. To this is added 20 ml. of trimethylorthobenzoate. The mixture is refluxed for 31 hours, then the solvents are evaporated giving a white solid which is washed twice with diethyl ether giving 3.0 gm. of white solid. This solid is combined with 50 ml. of diphenyl ether and heated with stirring in an oil bath at 265°-275° C. for 10 minutes. The mixture is cooled, petroleum ether is added and the mixture is filtered. The solid is washed twice with hot petroleum ether, giving 1.4 gm. of the desired product as a light tan solid, m.p. 292°-295° C.

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