反应详情

A mixture of Compound 4 (13.0 g, 86 mmol) and dimethylformamide dimethyl acetal (22.4 g, 188 mmol) was refluxed under nitrogen for 3 hrs. Solid precipitated from the reaction mixture. The reaction mixture was cooled, diluted with dichloromethane and ether (1:10, 200 mL). The solid was collected by filtration, triturated with a solution of dichloromethane and ether (1:20, 100 mL). Compound 5 was obtained as an orange solid (13.5 g, 65.4 mmol, 76%). GC/MS, m/z=206 at tR=13.39 min (100%). LC/MS, [M+H]′=207.

1. temperaturewas refluxed under nitrogen for 3 hrs
2. customSolid precipitated from the reaction mixture
3. temperatureThe reaction mixture was cooled
4. additiondiluted with dichloromethane and ether (1:10, 200 mL)
5. filtrationThe solid was collected by filtration
6. customtriturated with a solution of dichloromethane and ether (1:20, 100 mL)