反应详情

Into a reactor were introduced 110 g (0.60 mol) of the 1,1-diphenylethylene and 1,098 g of carbon tetrachloride under a nitrogen atmosphere. A solution prepared by mixing 95.9 g (0.60 mol) of bromine with 288 g of carbon tetrachloride was added dropwise thereto over 1 hour with cooling with ice. After completion of the addition, the reaction mixture was stirred at that temperature for 7 hours and then concentrated. To the residue were added 119 g of pyridine and 500 mL of toluene. This mixture was refluxed for 3 hours. After being cooled, the reaction mixture was washed with 5% hydrochloric acid and water, subsequently dried with anhydrous sodium sulfate, and then concentrated under reduced pressure. The resultant concentrate was distilled and then recrystallized from methanol to obtain 126 g (81%) of the target compound as white crystals.

1. customA solution prepared
2. additionwas added dropwise
3. temperatureover 1 hour with cooling with ice
4. additionAfter completion of the addition
5. concentrationconcentrated
6. additionTo the residue were added 119 g of pyridine and 500 mL of toluene
7. temperatureThis mixture was refluxed for 3 hours
8. temperatureAfter being cooled
9. washthe reaction mixture was washed with 5% hydrochloric acid and water
10. dry with materialsubsequently dried with anhydrous sodium sulfate
11. concentrationconcentrated under reduced pressure
12. concentrationThe resultant concentrate
13. distillationwas distilled
14. customrecrystallized from methanol