反应详情

The crude of 2-(chloromethyl)-3-(methoxycarbonyl)pyridine-1-oxide (20 g, 99.5 mmol) was added in small portion to POCl3 (200 g) at room temperature. The mixture was refluxed for 3 hours before it was concentrated in vacuo. The residue was poured into ice-water, neutralized with NaHCO3 solution, and extracted with AcOEt (125 mL×3). The combined organic layers were concentrated to give the crude title product (17 g, yield 78%), which was used in the next step reaction without further purification.

1. temperatureThe mixture was refluxed for 3 hours before it
2. concentrationwas concentrated in vacuo
3. additionThe residue was poured into ice-water
4. extractionextracted with AcOEt (125 mL×3)
5. concentrationThe combined organic layers were concentrated