反应详情

9,9-dihexyl-9H-fluorene (79 g, 236.2 mmol) and 2-bromo-2-methylpropanoyl bromide (54.3 g, 236.2 mmol) were injected into a 2000 mL round flask and then dissolved by adding 600 mL of carbon disulfide inputted thereto. Then, the reactor was cooled with ice water. Aluminum trichloride (78.7 g, 590.4 mmol) was slowly added thereto in ten lots over 2 hours under nitrogen atmosphere. Then, after the mixture was stirred at room temperature for 8 hours, the reaction was terminated by adding of 500 mL of distilled water, followed by washing with 500 mL of distilled water three times. The organic layer was dried over magnesium sulfate, followed by removal of volatile materials and drying, thereby obtaining 89.0 g of 9,9-dihexyl-2-methyl-2,3-dihydrocyclopenta[b]fluoren-1(9H)-one (yield: 93.6%) as highly viscous oil.

1. dissolutiondissolved
2. customthe reaction was terminated
3. additionby adding of 500 mL of distilled water
4. washby washing with 500 mL of distilled water three times
5. dry with materialThe organic layer was dried over magnesium sulfate
6. customfollowed by removal of volatile materials
7. customdrying