反応 #367623

反応方程式

sodium nitrite

N-(2-aminophenylsulfonyl)-N'-(4-methoxy-6-methyl-1,3,5-triazin-2-yl)urea

hydrochloric acid

sodium azide

→

N-(2-azidophenylsulfonyl)-N'-(4-methoxy-6-methyl-1,3,5-triazin-2-yl)urea

収率 27.3%

溶媒

water

water

反応条件

後処理

1. 1
   その他to rise to 20° C
2. 2
   抽出The reaction mixture is extracted with three 20 ml portions of methylene chloride
3. 3
   その他The combined organic phases are dried
4. 4
   濃縮concentrated
5. 5
   その他Recrystallisation of the residue

実験手順

A solution of 1 g of sodium nitrite in 4 ml of water is slowly added dropwise at 0°-5° C. to a mixture of 3.4 g of N-(2-aminophenylsulfonyl)-N'-(4-methoxy-6-methyl-1,3,5-triazin-2-yl)urea, 10 g of ice and 4 ml of 36% hydrochloric acid. After the reaction mixture has been stirred for 2 hours at 0° C., a solution of 1 g of sodium azide in 4 ml of water is added dropwise and the temperature is allowed to rise to 20° C. The reaction mixture is extracted with three 20 ml portions of methylene chloride. The combined organic phases are dried and concentrated. Recrystallisation of the residue yields 1.0 g of N-(2-azidophenylsulfonyl)-N'-(4-methoxy-6-methyl-1,3,5-triazin-2-yl)urea which decomposes at 175° C.

出典