反应详情

Under an atmosphere of argon, 9-bromo-10-(4-formylphenyl)anthracene (3.9 g, 11 mmole) and diethyl benzylphosphonate (3 g, 13 mmole, 1.2 eq) were suspended into DMSO (25 ml). To the resultant suspension, potassium t-butoxide (1.6 g, 14 mmole, 1.1 eq) was added and the obtained mixture was stirred at the room temperature for 10 hours and left standing for one night. The reaction mixture was diluted with water (50 ml) and subjected to extraction with toluene (300 ml). The organic layer was washed with water (50 ml) and a saturated aqueous solution of sodium chloride (50 ml) and dried with magnesium sulfate. Then, the solvent was removed by distillation and a yellow solid was obtained. The obtained solid was purified by recrystallization from toluene (40 ml) and yellow needle crystals (4.1 g, 86%) were obtained.

1. waitleft
2. waitstanding for one night
3. extractionsubjected to extraction with toluene (300 ml)
4. washThe organic layer was washed with water (50 ml)
5. dry with materiala saturated aqueous solution of sodium chloride (50 ml) and dried with magnesium sulfate
6. customThen, the solvent was removed by distillation
7. customa yellow solid was obtained
8. customThe obtained solid was purified by recrystallization from toluene (40 ml)