[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([F:23])=[C:6]([C:8]2[CH:13]=[CH:12][C:11]([CH2:14]O)=[CH:10][C:9]=2[C:16]2[C:20]([CH3:22])([CH3:21])[CH2:19][CH2:18][CH:17]=2)[CH:7]=1.CN(C=O)C.S(Cl)([Cl:31])=O>C(Cl)Cl>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([F:23])=[C:6]([C:8]2[CH:13]=[CH:12][C:11]([CH2:14][Cl:31])=[CH:10][C:9]=2[C:16]2[C:20]([CH3:22])([CH3:21])[CH2:19][CH2:18][CH:17]=2)[CH:7]=1To a stirred solution of 78.9B (0.048 g, 0.1 mmol) in DCM (2.00 mL) at 23° C. was added DMF (0.001 mL) followed by thionyl chloride (0.02 mL, 0.3 mmol). The reaction was stirred for one hour and then concentrated in vacuo. The product was purified on silica gel (0-10% EtOAc in hexanes) to yield 78.9C as a colorless oil (0.05 g, 99% yield).
Wird geladen…