反应详情

温度

85 °C

19 g of 2-propylpyridine-N-oxide were dissolved in 40 ml of glacial acetic acid/40 ml of acetic anhydride and stirred for 6 hours at 85° C. and 12 hours at ambient temperature. Excess anhydride was decomposed with H2O, the solution was neutralized with Na2CO3 and extracted with diethyl ether. After rotating in the ether phase, 12 g of 2-(1-acetoxypropyl)-pyridine remained. This product was dissolved in 120 ml of methanol (70%), mixed with 4 g of NaOH and refluxed for 6 hours. After rotating out the methanol mixing took place with water, extraction with diethyl ether and the organic phase was rotated in. 5.4 g of 2-(1-hydroxypropyl)-pyridine were left. 0.5 g of this substance was refluxed for 2 hours with 1 g of MnO2 and 30 ml of dichloromethane. After filtering off the MnO2, rotation in took place to dryness. 0.3 g of ethyl-2-pyridylketone was obtained.

1. extractionextracted with diethyl ether
2. dissolutionThis product was dissolved in 120 ml of methanol (70%)
3. additionmixed with 4 g of NaOH
4. temperaturerefluxed for 6 hours
5. extractionwith water, extraction with diethyl ether
6. wait5.4 g of 2-(1-hydroxypropyl)-pyridine were left
7. temperature0.5 g of this substance was refluxed for 2 hours with 1 g of MnO2 and 30 ml of dichloromethane
8. filtrationAfter filtering off the MnO2, rotation in took place to dryness