تفاعل #412919

معادلة التفاعل

tributyltin azide

ethyl cyanoformate

→

ethyl tetrazole-5-carboxylate

المذيبات

benzene

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةat reflux for 48 hours
2. 2
   أخرىThe benzene was removed under reduced pressure
3. 3
   workup.DISSOLUTIONthe residue was dissolved in an excess quantity of a dry solution of hydrogen chloride in ethanol
4. 4
   أخرىthe ethanol was removed in vacuo on the rotary evaporator
5. 5
   أخرىto give a red oil
6. 6
   غسيلChromatography of this oil on a column of silica gel, eluting with a mixture of methanol and chloroform (1:9 v/v)

الإجراء التجريبي

A solution of tributyltin azide (6.65 g) and ethyl cyanoformate (1.98 g) in dry benzene (25 ml) was heated at reflux for 48 hours. The benzene was removed under reduced pressure and the residue was dissolved in an excess quantity of a dry solution of hydrogen chloride in ethanol. The mixture was allowed to stand, and then the ethanol was removed in vacuo on the rotary evaporator to give a red oil. Chromatography of this oil on a column of silica gel, eluting with a mixture of methanol and chloroform (1:9 v/v), gave ethyl tetrazole-5-carboxylate, identical with samples prepared by the other methods as described above.

المصدر