反应详情

6-Bromo-4 methyl-3 pyridinamine (1.03 g, 5.51 mmol) was dissolved in DCM (20 ml) at 0° C. then added Hunig's Base (1.154 ml, 6.61 mmol) followed by pivaloyl chloride (0.745 ml, 6.06 mmol). After stirring for 1 hr, the reaction was not complete. Another equivalent of TEA and pivaloyl chloride were added then stirred for an hour. The reaction was poured into brine and extracted with DCM (2×). The organic layer was separated and dried over Na2SO4, filtered and concentrated. The residue was chromatographed thru a 200 g ISCO redisep column and eluted with 5% MeOH/DCM to yield title compound. LC-MS: M+2=273;

1. stirringthen stirred for an hour
2. extractionextracted with DCM (2×)
3. customThe organic layer was separated
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated
7. customThe residue was chromatographed thru a 200 g ISCO redisep column
8. washeluted with 5% MeOH/DCM