反応 #95219

反応方程式

5-amino-3-trichloromethyl-1,2,4-thiadiazole

3,5-dinitrobenzoyl chloride

→

pure product

収率 85.0%

5-(3,5-Dinitrobenzamido)-3-Trichloromethyl-1,2,4-Thiadiazole

収率 85.0%

溶媒

toluene

反応条件

後処理

1. 1
   その他The crude product precipitated from the reaction mixture
2. 2
   ろ過After isolation by filtration
3. 3
   洗浄the residue was washed with hot petroleum ether
4. 4
   その他finally recrystallized from methylene chloride

実験手順

A solution of 10.9 g (0.05 mole) 5-amino-3-trichloromethyl-1,2,4-thiadiazole and 12.6 g (0.055 mole) 3,5-dinitrobenzoyl chloride in 200 ml toluene was refluxed for 20 hours. The crude product precipitated from the reaction mixture upon cooling to -10° C. After isolation by filtration, the residue was washed with hot petroleum ether and finally recrystallized from methylene chloride to give 17.5 g (85% yield) of pure product; m.p. 197° C.

出典