反应详情

温度

25 °C

A solution of 52.3 g. of 9-carbamoylfluorene and 10 ml. of benzyltriethylammonium hydroxide in 700 ml. of tetrahydrofuran was heated at 45° C. for thirty minutes and then cooled to 25° C. The reaction mixture was diluted by addition in one portion of 25.2 g. of ethyl vinyl ketone. The reaction mixture was stirred at 25° C. for sixteen hours and at reflux for three hours. The mixture was cooled, added to 200 g. of ice and extracted with 50% ethyl acetate-diethyl ether. The organic extract was washed with water, with 10% sodium hydroxide, dried and the solvent was removed by evaporation under reduced pressure. The solid residue was crystallized from ethyl acetate and petroleum ether to afford 42.6 g of 9-carbamoyl-9-(3-oxopentyl)fluorene. m.p. 133°-135° C.

1. additionThe reaction mixture was diluted by addition in one portion of 25.2 g
2. temperatureat reflux for three hours
3. temperatureThe mixture was cooled
4. additionadded to 200 g
5. extractionof ice and extracted with 50% ethyl acetate-diethyl ether
6. extractionThe organic extract
7. washwas washed with water, with 10% sodium hydroxide
8. customdried
9. customthe solvent was removed by evaporation under reduced pressure
10. customThe solid residue was crystallized from ethyl acetate and petroleum ether