反应详情

To a mixture containing tert-butyl 5-(hydroxymethyl)pyridin-2-ylcarbamate (101; 4.5 g, 20.2 mmol) and DIPEA (16.0 g, 121 mmol) in THF (45 mL) was added MsCl (6.93 g, 60.5 mmol) over a period of 30 min at 0° C. The resulting reaction mixture was stirred at room temperature for 12 h. The mixture was then washed with water (2×5 mL), dried (Na2SO4) and concentrated under reduced pressure. The resulting residue was purified by chromatography (10:1 petroleum ether/ethyl acetate) to afford (6-(tert-butoxycarbonylamino)pyridin-3-yl)methyl methanesulfonate 102 (3.0 g, 61%).

1. customThe resulting reaction mixture
2. washThe mixture was then washed with water (2×5 mL)
3. dry with materialdried (Na2SO4)
4. concentrationconcentrated under reduced pressure
5. customThe resulting residue was purified by chromatography (10:1 petroleum ether/ethyl acetate)