반응 #319161

반응 방정식

product

2-[(1H-1,2,4-triazol-1yl)methyl]benzenesulfonamide

phenyl(4,6-dimethoxypyrimidin-2-yl)carbamate

DBU

→

subject compound

수율 70.7%

N-[(4,6-Dimethoxypyrimidin-2-yl)aminocarbonyl]-2-[(1H-1,2,4-triazol-2-yl)methyl]benzenesulfonamide

수율 70.7%

용매

p-dioxane

water

반응 조건

후처리

1. 1
   여과filtered
2. 2
   여과filtered
3. 3
   세척The residue was washed 2×10 ml water
4. 4
   기타suction-dried 16 hours
5. 5
   기타triturated with about 10 ml of warm ethyl acetate

실험 절차

By the procedure of Example 4, 0.4 g of the product of Example 7 was reacted with 0.52 g of phenyl(4,6-dimethoxypyrimidin-2-yl)carbamate and 0.26 g of "DBU" in 10 ml of p-dioxane. After stirring at 25° C. for two hours, the resulting suspension was diluted with about 50 ml of water, and filtered; the resulting filtrate was acidified with concentrated hydrochloric acid to pH 4, then filtered. The residue was washed 2×10 ml water, suction-dried 16 hours, then triturated with about 10 ml of warm ethyl acetate to yield 0.5 g of the subject compound; m.p. 219°-220° C. IR(nujol): 1690 cm-1 (c=o); NMR(CDCl3): ppm 3.9(S, 6H, OCH3); 5.8(S, 1H, py H); 6.0(S, 2H, CH2); 7.9 and 8.2(2S, 2H, tri 2H); 7.1-7.6(m, 4H, Ar+NH); 8.15(m, 1H, Ar).

출처