反应详情

A solution of 5.3 g (20 mmol) of 3,6-dibromo-1,2-phenylenediamine 1,4 g (19 mmol) of benzil 2b, 4.2 g of sodium acetate and 150 ml of glacial acetic acid were refluxed for 4 hours. The precipitate was filtered off, washed with 100 ml of water and recrystallized twice from dioxane. Drying under reduced pressure at 50° C. gave the pure product in the form of colorless crystals, which according to HPLC had a purity of about 99.5%. The yield was 6.45 g (73%).

1. filtrationThe precipitate was filtered off
2. washwashed with 100 ml of water
3. customrecrystallized twice from dioxane
4. customDrying under reduced pressure at 50° C.
5. customgave the pure product in the form of colorless crystals, which