反应详情

温度

190 °C

A mixture of 1-[2-(4-bromophenyl)propanoyl]pyrrolidine (140 mg, 0.5 mmol), 3-(trifluoromethyl)-4,5,6,7-tetrahydro-1H-indazole (95 mg, 0.5 mmol), copper (I) iodide (10 mol %, 10 mg, 0.05 mmol), N,N-dimethylglycine (20 mol %, 10 mg, 0.1 mmol) and potassium carbonate (138 mg, 1 mmol) in dimethylsulfoxide (2 ml) was stirred at 190° C. in a microwave reactor for a total of 1.5 h. The reaction mix was cooled and partitioned between ethyl acetate and water. The organic layer was dried over sodium sulphate and the solvent removed under reduced pressure. The resulting product was purified firstly by adding the material in dichloromethane to a 5 g pre-packed silica column and eluting with ethyl acetate, followed by mass directed auto-prep to give a crop of the title compound as a brown oil (8 mg, 4%).

1. additionThe reaction mix
2. temperaturewas cooled
3. custompartitioned between ethyl acetate and water
4. dry with materialThe organic layer was dried over sodium sulphate
5. customthe solvent removed under reduced pressure
6. customThe resulting product was purified firstly
7. additionby adding the material in dichloromethane to a 5 g pre-packed silica column
8. washeluting with ethyl acetate