反应详情

To a solution of 0.51 g (2.37 mmol) of 4,5-difluoroacridine (XIII) in 50 ml of 1,4-dioxane was added dropwise 9.3 ml (4.65 mmol) of a 0.5 M solution of potassium diphenylphosphide (Ph2P−K+) in tetrahydrofuran at room temperature. After the addition was completed, the mixture was heated at reflux for one hour. After cooling, 30 ml of distilled water was added to the brown reaction solution. The resulting precipitate was filtered off, washed thoroughly with distilled water, ethanol and n-pentane, and dried under high vacuum to obtain 1.02 g (79% of theory) of 4,5-bis(diphenylphosphino)acridine (Ia) as a yellow powder which will decompose from 255° C.

1. additionAfter the addition
2. temperaturethe mixture was heated
3. temperatureat reflux for one hour
4. temperatureAfter cooling
5. filtrationThe resulting precipitate was filtered off
6. washwashed thoroughly with distilled water, ethanol and n-pentane
7. customdried under high vacuum