[C:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1)(=[O:3])[CH3:2].CCCCOC[C:16]([C:18]1[CH:23]=[CH:22]C=CC=1)=[O:17].CC(C)([O-])C.[K+].[C:30](=O)([O:34]CC)[O:31][CH2:32][CH3:33]>O.C1(C)C=CC=CC=1>[CH2:16]([O:17][C:7]1[CH:8]=[CH:9][C:4]([C:1](=[O:3])[CH2:2][C:30]([O:31][CH2:32][CH3:33])=[O:34])=[CH:5][CH:6]=1)[CH2:18][CH2:23][CH3:22]The acetophenone (9.6 g, 0.05 mole) from (d) was added to a suspension of potassium t-butoxide (9.0 g, 0.08 mole) in diethyl carbonate (24.0 g, 0.2 mole) at 75° C. over 10 minutes. Toluene (40 ml) was added to keep the suspension mobile and heating at 95° C. continued for 30 minutes. After cooling to 50° C., the suspension was poured into cold water (500 ml) and extracted with ethyl acetate (300 ml). The organic solution was dried and evaporated under reduced pressure to give the product (13.2 g, 95%) as a dark red liquid which was used in the next reaction without further purification.
Loading…
