反应详情

温度

86 °C

To a solution of 4-methylaminomethylpiperidine-1-carboxylic acid tert-butyl ester (41 mg, 0.18 mmol) in anhydrous DMF (3 mL) was added 4-bromo-2-pyridin-4-yl-pyrimidine (Preparation 1, 42 mg, 0.18 mmol) and DIPEA (63 μL, 0.36 mmol), then the resulting solution was heated to 86° C. (bath) for 6 h. The reaction mixture was cooled to 20° C., then H2O (20 mL) and EtOAc (10 mL) were added. The layers were separated then the aqueous phase was extracted with EtOAc (2×30 mL). The combined organics were washed with brine (30 mL), dried (MgSO4), filtered and concentrated in vacuo. Flash column chromatography (EtOAc) gave the title compound: RT=2.87 nm in; m/z (ES+)=384 [M+H]+.

1. temperatureThe reaction mixture was cooled to 20° C.
2. customThe layers were separated
3. extractionthe aqueous phase was extracted with EtOAc (2×30 mL)
4. washThe combined organics were washed with brine (30 mL)
5. dry with materialdried (MgSO4)
6. filtrationfiltered
7. concentrationconcentrated in vacuo