反应详情

A mixture of 4.1 g (0.0155 mol) of 2-(1,4-dioxa-8-azaspiro[4.5]decan-8-yl]pyrimidine-4-carboxamide, 41 ml of acetic acid and 4.1 ml of concentrated hydrochloric acid is heated at reflux temperature for 30 minutes. The mixture is concentrated under reduced pressure, the residue is then taken up in a mixture of dichloromethane and water, is alkalified with aqueous ammonia solution, extracted with dichloromethane, the organic phase is dried over magnesium sulphate, filtered and the solvent evaporated under reduced pressure. 3 g of compound are obtained.

1. temperatureis heated
2. temperatureat reflux temperature for 30 minutes
3. concentrationThe mixture is concentrated under reduced pressure
4. additionthe residue is then taken up in a mixture of dichloromethane and water
5. extractionextracted with dichloromethane
6. dry with materialthe organic phase is dried over magnesium sulphate
7. filtrationfiltered
8. customthe solvent evaporated under reduced pressure