反应详情

13.0 g (44 mmol) 5-acetyl-7-benzyloxy-3,4-dihydro-1H-quinolin-2-one are suspended in 130 mL dioxane and combined with 15.0 g (66 mmol) 2,3-dichloro-5,6-dicyanobenzoquinone. The mixture is refluxed for 30 minutes, cooled to ambient temperature and stirred for a further 2 hours. The solid is filtered off, washed with dioxane and dissolved in 600 mL dichloromethane/methanol (9:1). The solution is washed with sodium hydrogen carbonate solution, dried with sodium sulphate and evaporated down. Then the residue is suspended in methanol, filtered and dried.

1. temperatureThe mixture is refluxed for 30 minutes
2. filtrationThe solid is filtered off
3. washwashed with dioxane
4. dissolutiondissolved in 600 mL dichloromethane/methanol (9:1)
5. washThe solution is washed with sodium hydrogen carbonate solution
6. dry with materialdried with sodium sulphate
7. customevaporated down
8. filtrationfiltered
9. customdried