تفاعل #4258

معادلة التفاعل

dicyclohexylcarbodiimide

1-(3-carboxyphenyl)-5-mercaptotetrazole

4-(2-formylhydrazino)aniline

→

desired compound

المردود 25.4%

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

المردود 25.4%

المذيبات

dimethylformamide

dimethylformamide

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONAfter the addition
2. 2
   أخرىThe 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
   ترشيحThe thus precipitated crystals were filtered
6. 6
   غسيلwashed with water
7. 7
   workup.ADDITIONdispersed in 100 ml of hot methanol
8. 8
   درجة الحرارةto cool to room temperature
9. 9
   ترشيحfiltered
10. 10
    غسيلThe filtrate was washed with methanol

الإجراء التجريبي

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).

المصدر