반응 #4258

반응 방정식

dicyclohexylcarbodiimide

1-(3-carboxyphenyl)-5-mercaptotetrazole

4-(2-formylhydrazino)aniline

→

desired compound

수율 25.4%

5-Mercapto-1-{3-[4-(2-Formylhydrazino)Phenylcarbamoyl]Phenyl}Tetrazole

수율 25.4%

용매

dimethylformamide

dimethylformamide

반응 조건

후처리

1. 1
   workup.ADDITIONAfter the addition
2. 2
   기타The precipitated dicyclohexylurea was separated by filtration
3. 3
   workup.ADDITIONthe filtrate was added to 500 ml of ice-water
4. 4
   workup.STIRRINGwhile stirring
5. 5
   여과The thus precipitated crystals were filtered
6. 6
   세척washed with water
7. 7
   workup.ADDITIONdispersed in 100 ml of hot methanol
8. 8
   온도to cool to room temperature
9. 9
   여과filtered
10. 10
    세척The filtrate was washed with methanol

실험 절차

In 50 ml of dimethylformamide were dissolved 11.1 g of 1-(3-carboxyphenyl)-5-mercaptotetrazole and 7.6 g of 4-(2-formylhydrazino)aniline, and a solution of 10.3 g of dicyclohexylcarbodiimide in 10 ml of dimethylformamide was added dropwise to the solution at 0° C. in a nitrogeneous atmosphere over about 30 minutes. After the addition, the mixture was stirred at room temperature for 3 hours. The precipitated dicyclohexylurea was separated by filtration, and the filtrate was added to 500 ml of ice-water while stirring. The thus precipitated crystals were filtered, washed with water and dispersed in 100 ml of hot methanol. The dispersion was allowed to cool to room temperature and filtered. The filtrate was washed with methanol to obtain 4.5 g of the desired compound. Melting point: 202° C. (with decomposition).

출처