反应详情

To a solution of 5-Bromo-6-chloro-pyridine-3-sulfonic acid (2-hydroxy-1-hydroxymethyl-1-methyl-ethyl)-amide (550 mg, 2 mmol) in MeOH (5 mL) was added a solution of sodium methoxide (c=5.4 mol/L in MeOH, 10 mmol) at rt for 48 h. The reaction mixture was poured into a 1N solution of HCl and was extracted with 2 portions of EtOAc, dried over Na2SO4, filtered, concentrated, and purified by column chromatography (heptane/EtOAc, 1:1) to give the title compound (0.28 g, 51%) as a white solid. MS (ISN) 353.1 [(M−H)−], 355.1 [(M+2−H)−].

1. extractionwas extracted with 2 portions of EtOAc
2. dry with materialdried over Na2SO4
3. filtrationfiltered
4. concentrationconcentrated
5. custompurified by column chromatography (heptane/EtOAc, 1:1)