反应详情

197 g of 1A was placed in a flask, which then was purged with nitrogen, and a slow stream of nitrogen was passed through the system while the 1A was heated gradually. At about 160° C., an exothermic reaction began, and the temperature rose to 220° C. The mixture was contained with cooling, then heated at 185°-200° C. for 1.5 hours, diluted with ether, and filtered. The solvent was evaporated from the filtrate to give crude 2-(1-methyl-2-propenyl)-3-methyl-6-nitrophenol (1B), as a dark syrup.

1. customwhich then was purged with nitrogen
2. temperaturewas heated gradually
3. customAt about 160° C., an exothermic reaction
4. customrose to 220° C
5. temperaturewith cooling
6. temperatureheated at 185°-200° C. for 1.5 hours
7. filtrationfiltered
8. customThe solvent was evaporated from the filtrate