反应详情

In 20 ml of DMF were dissolved 2.0 g (5.8 mmol) of 3,7-diformyl-10-p-tolylphenothiazine (2b) and 4.0 g (13.2 mmol) of diethyl diphenylmethylphosphonate (3a). Thereto was gradually added 1.5 g (13.4 mmol) of potassium t-butoxide. After the mixture was reacted overnight, 10 ml of methanol was added thereto. The crystals precipitated were taken out by filtration, dissolved in chloroform, purified by silica gel column chromatography (toluene), and then recrystallized from a chloroform/hexane mixed solvent to obtain 1.48 g of the target compound.

1. customAfter the mixture was reacted overnight
2. customThe crystals precipitated
3. filtrationwere taken out by filtration
4. dissolutiondissolved in chloroform
5. custompurified by silica gel column chromatography (toluene)
6. customrecrystallized from a chloroform/hexane mixed solvent