反应详情

To a solution of tert-butyl 5-(hydroxymethyl)pyridin-2-ylcarbamate 116 (85.0 g, 379 mmol) and diisopropylethylamine (296 g, 2.27 mol) in THF (850 mL) was added methanesulfonyl chloride (130 g, 1.14 mol) over a period of 30 min at 0° C. The mixture was stirred for 12 h at room temperature then washed with H2O (2×100 mL) and dried over Na2SO4. The mixture was concentrated and the crude residue was purified by flash chromatography (petroleum ether: ethyl acetate=10:1) to give 117 (30 g, 63% yield).

1. washthen washed with H2O (2×100 mL)
2. dry with materialdried over Na2SO4
3. concentrationThe mixture was concentrated
4. customthe crude residue was purified by flash chromatography (petroleum ether: ethyl acetate=10:1)