反应详情

温度

-78 °C

A solution of 9-(3-methoxyphenyl)-3,6-dibromo-9H-carbazole (26 g, 1 eq) in dry THF (700 ml) is admixed slowly at −78° C. under argon with n-butyllithium (1.6 M in hexane, 41 ml, 1 eq) and stirred at −78° C. for 2 h. After a solution of chlorotriphenylsilane (30 g, 1.5 eq) in dry THF (150 ml) had been added at −78° C., the mixture was warmed to room temperature overnight with stirring. Excess butyllithium is hydrolyzed with saturated ammonium chloride solution. The precipitated reaction product is filtered off and washed thoroughly with methylene chloride. The combined methylene chloride filtrates are extracted with water and concentrated to dryness. The residue is stirred with acetone and filtered off. Yield 74%.

1. temperaturethe mixture was warmed to room temperature overnight
2. stirringwith stirring
3. customThe precipitated reaction product
4. filtrationis filtered off
5. washwashed thoroughly with methylene chloride
6. extractionThe combined methylene chloride filtrates are extracted with water
7. concentrationconcentrated to dryness
8. stirringThe residue is stirred with acetone
9. filtrationfiltered off