反应详情

A mixture of 6-bromo-3-methoxypyridin-2-amine (10.2 g, 50.2 mmol), Boc2O (38.2 g, 0.18 mol) and 4-(dimethylamino)pyridine (1.2 g, 9.82 mmol) in MeCN (550 mL) was refluxed for 2 h. After cooling to rt and concentration in vacuo EtOAc (500 mL) was added and the organic phase washed with water (100 mL) and brine (50 mL). The organic phase was dried (MgSO4), filtered and the filtrate concentrated in vacuo. Purification by chromatography eluting with 4:1 DCM-heptane yielded a mixture of the title compound and di-tert-butyl(6-bromo-3-methoxypyridin-2-yl)imidodicarbonate (10.6 g) in an approximate ratio of 55:45.

1. temperaturewas refluxed for 2 h
2. concentrationconcentration in vacuo EtOAc (500 mL)
3. additionwas added
4. washthe organic phase washed with water (100 mL) and brine (50 mL)
5. dry with materialThe organic phase was dried (MgSO4)
6. filtrationfiltered
7. concentrationthe filtrate concentrated in vacuo
8. customPurification by chromatography
9. washeluting with 4:1 DCM-heptane
10. customyielded