반응 #58075

반응 방정식

sodium

ethyl acetimidate hydrochloride

4-methyl-benzoic acid hydrazide

→

solid

수율 15.7%

4-methyl-benzoic acid-(1-imino-ethyl)-hydrazide

수율 15.7%

용매

ethanol

ethanol

반응 조건

후처리

1. 1
   여과the precipitated sodium chloride is filtered off
2. 2
   기타The reaction mixture is evaporated down
3. 3
   온도cooled
4. 4
   여과The precipitated solid is filtered off
5. 5
   세척washed with cold ethanol and diethyl ether (5.7 g white solid)

실험 절차

1.65 g (72 mmol) sodium are dissolved in 80 mL ethanol. 8.89 g (72 mmol) ethyl acetimidate hydrochloride in 160 mL ethanol are added at ambient temperature and the precipitated sodium chloride is filtered off. The filtrate is combined with 6.00 g (40 mmol) 4-methyl-benzoic acid hydrazide and stirred overnight. The reaction mixture is evaporated down and cooled. The precipitated solid is filtered off and washed with cold ethanol and diethyl ether (5.7 g white solid). A further 1.2 g solid are obtained from the filtrate after distillation of the solvents and recrystallisation from ethanol.

출처