Reaktion #5018

Reaktionsgleichung

3-oxabicyclo[3.2.2]-nonan-2,4-dione

1-(4-aminobutyl)-4-(2-pyrimidinyl) piperazine

3-oxabicyclo[3.2.2]nonan-2,4-dione

3-oxabicyclo[3.2.2]nonan-2,4-dione

→

title compound

Ausbeute 8.7%

3-(4-[4-(2-Pyrimidinyl)-1-piperazinyl]butyl)-3-azabicyclo[3.2.2]nonan-2,4-dione

Ausbeute 8.7%

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas heated in an oil bath at 220°-230° C. for 15 minutes
2. 2
   TemperaturHeating in an oil bath at 220°-230° C.
3. 3
   TemperaturHeating
4. 4
   workup.WAITwas continued for 30 minutes at 220°-230° C.
5. 5
   Temperaturthe reaction mixture was cooled
6. 6
   SonstigeThe resulting product was chromatographed on silica gel
7. 7
   Wascheneluting with dichloromethane/methanol (96:4 followed by 94:6)

Vorschrift

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).

Quelle