反应详情

温度

100 °C

A mixture of 3,5-dimethyl-4-nitrosophenol (70.63 g) from above and (NH4)6Mo7O24.4H2O) (2.83g) in 770 ml of glacial acetic acid was warmed to 100° C. 30% H2O2 (84 ml) was added to the mixture in 10 ml portions until an exothermic reaction was observed. The reaction mixture was then stirred and the remainder of the H2O2 solution added in small portions. The reaction mixture was heated and stirred until a clear dark red solution results. A yellow-orange solid precipitated from the solution after stirring for another 20-30 minutes. The reaction mixture was stirred overnight and filtered to give a small amount of a yellow solid and a clear dark red filtrate. The red filtrate was concentrated in vacuo and partitioned between water and ether. The aqueous layer was washed with ether and the combined ether extracts washed with 10% sodium carbonate until the aqueous layer becomes basic. The ether extract was dried over anhydrous sodium sulfate, filtered, concentrated and allowed to cool overnight. After cooling in an ice bath the mixture was filtered to give 49.5 g of 3,5-dimethyl-4-nitrophenol as a yellow-green solid. Mp. 106-108° C.

1. temperatureThe reaction mixture was heated
2. stirringstirred until a clear dark red solution
3. customresults
4. customA yellow-orange solid precipitated from the solution
5. stirringafter stirring for another 20-30 minutes
6. stirringThe reaction mixture was stirred overnight
7. filtrationfiltered
8. customto give a small amount of a yellow solid
9. concentrationThe red filtrate was concentrated in vacuo
10. custompartitioned between water and ether
11. washThe aqueous layer was washed with ether
12. washthe combined ether extracts washed with 10% sodium carbonate until the aqueous layer
13. extractionThe ether extract
14. dry with materialwas dried over anhydrous sodium sulfate
15. filtrationfiltered
16. concentrationconcentrated
17. temperatureto cool overnight
18. temperatureAfter cooling in an ice bath the mixture
19. filtrationwas filtered