反应详情

温度

90 °C

Add tetrakistriphenylphosphine palladium(0) (27 mg, 0.024 mmol), cesium fluoride (143 mg, 0.942 mmol) and 5-methyl-thiophen-2-yl-boronic acid (134 mg, 0.942 mmol) to a stirred solution of 7-chloro-3-(2,2,2-trifluoroacetyl)-6-trifluoromethanesulfonyloxy-2,3,4,5-tetrahydro-1H-benzo[d]azepine (200 mg, 0.471 mmol) in anhydrous DME (8 mL) at room temperature. Heat at 90° C. overnight. Cool the reaction mixture to room temperature, dilute with EtOAc and wash with water. Extract the aqueous phase twice with EtOAc. Dry the combined organic extracts over Na2SO4, filter and concentrate in vacuo. Purify the crude mixture by chromatography on silica gel eluting with hexane/EtOAc (1:0 and 19:1) to obtain 7-chloro-6-(5-methyl-thiophen-2-yl)-3-(2,2,2-trifluoroacetyl)-2,3,4,5-tetrahydro-1H-benzo[d]azepine (124 mg, 70%).

1. temperatureCool the reaction mixture to room temperature
2. washwash with water
3. extractionExtract the aqueous phase twice with EtOAc
4. dry with materialDry the combined organic extracts over Na2SO4
5. filtrationfilter
6. concentrationconcentrate in vacuo
7. customPurify the crude mixture by chromatography on silica gel eluting with hexane/EtOAc (1:0 and 19:1)