反応 #319159

反応方程式

hydrochloric acid

sulfonamide

2-[[5-(Methylthio)-1,3,4-thiadiazol-2-yl]methyl]benzenesulfonamide

phenyl(4-methoxy-6-methyl-1,3,5-triazin-2-yl)carbamate

DBU

→

subject compound

収率 32.2%

N-[(4-Methoxy-6-methyl-1,3,5-triazin-2-yl)aminocarbonyl]-2-[[5-(methylthio)-1,3,4-thiadiazol-2-yl]methyl]-benzenesulfonamide

収率 32.2%

溶媒

water

p-dioxane

反応条件

後処理

1. 1
   ろ過filtration
2. 2
   洗浄the residue was washed with water (2×20ml)
3. 3
   乾燥with ether (1×20ml) and suction-dried

実験手順

By the procedure of Example 4, 0.3 g of the sulfonamide prepared in Example 3 was reacted with 0.29 g of phenyl(4-methoxy-6-methyl-1,3,5-triazin-2-yl)carbamate and 0.15 g of "DBU" in 10 ml of p-dioxane. After stirring two hours at room temperature the solution was diluted with about 75 ml of water and acidified with concentrated hydrochloric acid (red to litmus paper). Following filtration, the residue was washed with water (2×20ml) then with ether (1×20ml) and suction-dried to give 0.15 g of the subject compound; m.p. 140°-146° C. NMR (CDCl3): δ2.6(d,6H,SCH3, OCH3); 4.1 (S, 3H, CH3); 4.9(S, 2H, CH2); 7.4-7.7(m, 4H, Ar+NH); 8.3(d, 1H, Ar).

出典