反应详情

A suspension of 430 mg (1.5 mmol) of ethyl 5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a]thieno[2,3-f][1,4]-diazepine-3-carboxylate and 99 mg (1.5 mmol) of potassium cyanide in 15 ml of absolute methanol is heated under reflux for 3 hours while stirring. After evaporation in vacuo, the residue is treated with ca 20 ml of ice/water and extracted three times with ca 30 ml of chloroform each time. The combined chloroform phases are washed twice with ca 20 ml of water each time, dried over magnesium sulphate and evaporated. After washing with boiling ethyl acetate, there is obtained methyl 5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a]thieno[2,3-f][1,4]diazepine-3-carboxylate of melting point 244°-245° C.

1. temperatureis heated
2. temperatureunder reflux for 3 hours
3. customAfter evaporation in vacuo
4. additionthe residue is treated with ca 20 ml of ice/water
5. extractionextracted three times with ca 30 ml of chloroform each time
6. washThe combined chloroform phases are washed twice with ca 20 ml of water each time
7. dry with materialdried over magnesium sulphate
8. customevaporated
9. washAfter washing with boiling ethyl acetate