反应详情

5-{[(3-Methoxyphenyl)amino]methylene}-2,2-dimethyl-1,3-dioxane-4,6-dione (Intermediate 11, 43.5 g, 157 mmol) was added in small portions to phenylether (200 mL) at 225-260° C. under stirring. The reaction mixture was stirred for an additional 5 minutes, until the evolution of gas had stopped. The reaction mixture was cooled to room temperature and the precipitate was collected by filtration and washed with hexanes. Purification by recrystallization from methanol gave 12.4 g (45% yield) of product as a green solid, mp 210° C.

1. stirringThe reaction mixture was stirred for an additional 5 minutes, until the evolution of gas
2. filtrationthe precipitate was collected by filtration
3. washwashed with hexanes
4. customPurification
5. customby recrystallization from methanol