反应详情

A solution of 30.0 grams of phloroglucinol and 70 milliliters of pyridine in 300 milliliters of dichloromethane was stirred at room temperature under a nitrogen atmosphere. Thereafter, a solution of 8.0 grams of (4-chloroformyl-9-fluorenylidene)malononitrile in 400 milliliters of dichloromethane was added thereto over a period of 1 hour. After addition, the reaction mixture was further stirred for another hour. The mixture was washed three times dilute aqueous HCl solution, twice with dilute aqueous NaHCO3 solution, and once with water. The solution was dried, filtered, and evaporated under reduced pressure to give the crude product. Recrystallization from methanol afforded 6.1 grams of (b), mp., 255.5° to 257° C.

1. additionAfter addition
2. washThe mixture was washed three times dilute aqueous HCl solution
3. customThe solution was dried
4. filtrationfiltered
5. customevaporated under reduced pressure
6. customto give the crude product
7. customRecrystallization from methanol