反应详情

Methylsulfonylchloride (0.031 ml, 0.39 mmol) was added dropwise to a solution of Compound B (0.070 g, 0.27 mmol) and DIEA (0.14 ml, 0.80 mmol) in methylene chloride (2 ml) at -78° C. The mixture was allowed to warm slowly to room temperature and was stirred at rt for 16h. The mixture was quenched with 10% NaHCO3 (10 ml) and the solution was extracted with methylene chloride (3×10 ml). The combined organic layers were dried (Na2SO4), filtered and concentrated under vacuum. The residue was purified by flash chromatography (19/1 methylene chloride/iPrOH) to afford Compound C (0.064 g, 85%) as a solid. MS (M+H)+ 343

1. customThe mixture was quenched with 10% NaHCO3 (10 ml)
2. extractionthe solution was extracted with methylene chloride (3×10 ml)
3. dry with materialThe combined organic layers were dried (Na2SO4)
4. filtrationfiltered
5. concentrationconcentrated under vacuum
6. customThe residue was purified by flash chromatography (19/1 methylene chloride/iPrOH)