[Cl:1][C:2]1[CH:3]=[C:4](B(O)O)[CH:5]=[CH:6][CH:7]=1.C([O-])(=O)C.C([O-])(=O)C.[Cl:19][C:20]1[CH:21]=[C:22]([I+2:26])[CH:23]=[CH:24][CH:25]=1.[F:27][B-:28]([F:31])([F:30])[F:29].[Na+]>C(Cl)Cl>[F:27][B-:28]([F:31])([F:30])[F:29].[Cl:1][C:2]1[CH:3]=[C:4]([I+:26][C:22]2[CH:23]=[CH:24][CH:25]=[C:20]([Cl:19])[CH:21]=2)[CH:5]=[CH:6][CH:7]=1Borontrifluoride diethyl etherate (16.51 g, 116.3 mmol) was added slowly to 3-chlorophenyl boronic acid (17.37 g, 111.0 mmol) in DCM (170 mL) at −5° C., while stirring. After 15 minutes, the title compound of Example 15.1 (37.71 g, 105.8 mmol) in DCM (150 mL) was added slowly. The reaction stirred for 1 h at 0° C. and sodium tetrafluoroborate (225 g in 300 mL water) was added and stirred for 1 h. The organic layer was separated, dried over sodium sulphate, filtered and concentrated and triturated with ether to afford the title product (31.6 g, 68%) as a light brown solid.
Wird geladen…
