反应详情

温度

110 °C

A mixture of 3-(4-chloropyrimidin-2-yl)-5-(2,6-difluorophenyl)-1-tosyl-1H-indole (500 mg, 10 mmol) and (R)-tert-butyl 3-aminopiperidine-1-carboxylate (404 mg, 2.02 mmol) in DMSO (10 mL) was heated at 110° C. for 12 h. The resulting mixture was cooled to at RT for 2 h. The reaction mixture was quenched with ice cold water and extracted with EtOAc. The organic layer was dried over Na2SO4, filtered and concentrated to yield crude compound. Purification by silica gel column chromatography, eluting with 5-15% EtOAc and hexanes to the title compound (500 mg, 75%). MS (ESI, pos. ion) m/z: 660 (M+1).

1. temperatureThe resulting mixture was cooled to at RT for 2 h
2. customThe reaction mixture was quenched with ice cold water
3. extractionextracted with EtOAc
4. dry with materialThe organic layer was dried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated
7. customto yield crude compound
8. customPurification by silica gel column chromatography
9. washeluting with 5-15% EtOAc and hexanes to the title compound (500 mg, 75%)