反应详情

Combine 7-chloro-3-(2,2,2-trifluoroacetyl)-6-trifluoromethanesulfonyloxy-2,3,4,5-tetrahydro-1H-benzo[d]azepine (200 mg, 0.47 mmol), 3-biphenylboronic acid (280 mg, 1.4 mmol), tetrakis(triphenylphosphine)palladium(0) (54 mg, 0.047 mmol) and cesium fluoride (144 mg, 0.94 mmol) in anhydrous DME (8 mL) and reflux the mixture for 3 h. Cool the reaction mixture and partition between brine and EtOAc. Dry the organic layer over Na2SO4, filter and concentrate in vacuo. Purify the crude mixture by chromatography on silica gel eluting with hexane/EtOAc (1:0 to 7:3 gradient) to obtain 6-(biphenyl-3-yl)-7-chloro-3-(2,2,2-trifluoroacetyl)-2,3,4,5-tetrahydro-1H-benzo[d]azepine.

1. temperatureCool the reaction mixture
2. custompartition between brine and EtOAc
3. dry with materialDry the organic layer over Na2SO4
4. filtrationfilter
5. concentrationconcentrate in vacuo
6. customPurify the crude mixture by chromatography on silica gel eluting with hexane/EtOAc (1:0 to 7:3 gradient)