反应详情

An intimate mixture of 0.5 g (2.14 mmol) of 1-(4-aminobutyl)-4-(2-pyrimidinyl) piperazine and 0.22 g (1.42 mmol) of 3-oxabicyclo[3.2.2]nonan-2,4-dione was heated in an oil bath at 220°-230° C. for 15 minutes. An additional 0.22 g (1.42 mmol) of 3-oxabicyclo[3.2.2]nonan-2,4-dione was added. Heating in an oil bath at 220°-230° C. was continued for 15 minutes and then an additional 0.22 g (1.42 mmol) of 3-oxabicyclo[3.2.2]-nonan-2,4-dione was added. Heating was continued for 30 minutes at 220°-230° C. and then the reaction mixture was cooled. The resulting product was chromatographed on silica gel, eluting with dichloromethane/methanol (96:4 followed by 94:6), to give 46 mg of the title compound (6% yield).

1. temperaturewas heated in an oil bath at 220°-230° C. for 15 minutes
2. temperatureHeating in an oil bath at 220°-230° C.
3. temperatureHeating
4. waitwas continued for 30 minutes at 220°-230° C.
5. temperaturethe reaction mixture was cooled
6. customThe resulting product was chromatographed on silica gel
7. washeluting with dichloromethane/methanol (96:4 followed by 94:6)