反应详情

温度

120 °C

To 5-Iodo-2-methoxy-3-(trifluoromethyl)pyridine (0.97 g, 3.20 mmol) (ECA International Product List) was added DMF (8.0 mL), (9,9-dimethyl-9H-xanthene-4,5-diyl)bis(diphenylphosphine) (0.093 g, 0.160 mmol), Pd2(dba)3 (0.147 g, 0.160 mmol), diphenylmethanimine (0.806 mL, 4.80 mmol), and sodium 2-methylpropan-2-olate (1.231 g, 12.80 mmol), and the resulting mixture was heated at 120° C. for 30 min. The reaction mixture was then diluted with 100 mL of EtOAc, added to a separatory funnel, partitioned with 1 N HCl (aqueous), and washed 2 times with 50 mL of sodium bicarbonate (saturated, aqueous). The organic layer was separated, dried over sodium sulfate, and concentrated in vacuo. Chromatographic purification of the residue (silica gel, 0% to 5% (2 M ammonia in MeOH)/DCM) provided the title compound (34% yield). m/z (ESI, +ve ion) 193.2 (M+H)+.

1. additionadded to a separatory funnel
2. custompartitioned with 1 N HCl (aqueous)
3. washwashed 2 times with 50 mL of sodium bicarbonate (saturated, aqueous)
4. customThe organic layer was separated
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated in vacuo
7. customChromatographic purification of the residue (silica gel, 0% to 5% (2 M ammonia in MeOH)/DCM)