反应详情

温度

120 °C

To a solution of methyl 3-(6-chloro-3-methylpicolinamido)-2,4-dimethylbenzoate (0.50 g, 0.0015 mol), tert-butyl-dimethyl-(4-piperidyloxy)silane (0.90 g, 0.0045 mol) and Cs2CO3 (2.00 g, 0.006 mol) in toluene (6 ml) is added Pd2(dba)3 (0.14 g, 0.00015 mol) followed by BINAP (0.086 g, 0.00015 mol). The reaction mixture is purged with nitrogen for 5 minutes and then heated at 120° C. After 4 hours, the reaction is cooled to ambient temperature, filtered through Celite™, and washed with EtOAc. The combined filtrate is dried over sodium sulfate, filtered, and concentrated under reduced pressure to afford the title compound as a white semi-solid (0.220 g, 29%). Mass spectrum (m/z): 398.2 (M+1).

1. customThe reaction mixture is purged with nitrogen for 5 minutes
2. temperaturethe reaction is cooled to ambient temperature
3. filtrationfiltered through Celite™
4. washwashed with EtOAc
5. dry with materialThe combined filtrate is dried over sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure