反应详情

A mixture of 25 g of 2-hydroxy-4-methyl-3-nitropyridine, 12.5 g of phosphorous pentachloride, and 62 ml of phosphorous oxychloride was refluxed for 2 hrs. After cooling, the mixture was poured onto crashed ice and stirred until a precipitate formed. The product was extracted with methylene chloride, dried (sodium sulfate) and concentrated to a brown oil, which was washed with hot hexane. Concentration in vacuo provided 16.2 g of the the title compound, m.p. 45°-47° C.

1. temperaturewas refluxed for 2 hrs
2. temperatureAfter cooling
3. additionthe mixture was poured
4. customformed
5. extractionThe product was extracted with methylene chloride
6. dry with materialdried (sodium sulfate)
7. concentrationconcentrated to a brown oil, which
8. washwas washed with hot hexane
9. concentrationConcentration in vacuo