[O:1]=[C:2]1[C:7]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)=[CH:6][O:5][C:4]([C:14]([NH2:16])=O)=[CH:3]1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.Cl.C(Cl)(Cl)Cl>C(Cl)(Cl)(Cl)Cl.C(Cl)Cl.C(N(CC)CC)C>[O:1]=[C:2]1[C:7]([C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=2)=[CH:6][O:5][C:4]([C:14]#[N:16])=[CH:3]1A suspension of this amide (3.5 g) and triphenylphosphine (8.54 g) in carbon tetrachloride (10 ml), methylene chloride (20 ml) and triethylamine (2.3 ml) was stirred for 4 hours at room temperature. Ice (60 g) and 2 N hydrochloric acid (30 ml) were added, followed by sufficient chloroform to dissolve all the solid material. The solvent layer was washed with water, dried and evaporated, and the residue was crystallised from chloroform-petroleum spirit (60°-80° C.) and then from ethanol to give the title product (mp 177°-179° C.).
Wird geladen…
