反应详情

To a flask equipped with condenser, stirrer, under nitrogen, was added 3,6-dimethyl-4,5-dichloronitrobenzene (50 g, 0.23 mol), 2,4-dimethylphenol (38.5 g, 0.32 mol), potassium carbonate (50 g, 0.36 mol), and dimethylformamide (125 ml). The resulting mixture was heated at 90°~100° for 72 hours. It was then cooled, filtered, and concentrated to give dark oil. It was partitioned between toluene (300 ml) and 4% sodium hydroxide (250 ml) and then separated. The organic layer was washed with water and brine, dried (Na2SO4) and concentrated to give dark oil. Solid was formed after the oil was trituated with hexane. The solid was washed with cold hexane and vacuum dried to give a tan powder (47.8 g, 0.16 mol); mp 78°~80°.

1. customTo a flask equipped with condenser, stirrer, under nitrogen
2. temperatureThe resulting mixture was heated at 90°~100° for 72 hours
3. temperatureIt was then cooled
4. filtrationfiltered
5. concentrationconcentrated
6. customto give dark oil
7. customIt was partitioned between toluene (300 ml) and 4% sodium hydroxide (250 ml)
8. customseparated
9. washThe organic layer was washed with water and brine
10. dry with materialdried (Na2SO4)
11. concentrationconcentrated
12. customto give dark oil
13. customSolid was formed after the oil
14. washThe solid was washed with cold hexane and vacuum
15. customdried