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 crushed 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. customonto crushed ice
5. customformed
6. extractionThe product was extracted with methylene chloride
7. dry with materialdried (sodium sulfate)
8. concentrationconcentrated to a brown oil, which
9. washwas washed with hot hexane
10. concentrationConcentration in vacuo