反应详情

Methanesulfonyl chloride (20 μL; 0.26 mmol; 1.2 eq.) was added to a solution of Example 69 (83 mg; 0.22 mmol; 1 eq.) in pyridine (1 mL) and the resulting solution was stirred at room temperature for 16 hours. The solution was then partitioned between water and ethyl acetate. The two phases were separated and the aqueous layer was extracted with ethyl acetate. The combined organic phase was washed (3×) with 0.1M HCl, dried over magnesium sulfate and concentrated in vacuo. Purification by column chromatography (c-hexane/ethyl acetate, 60/40) afforded the title compound as a white solid.

1. customThe solution was then partitioned between water and ethyl acetate
2. customThe two phases were separated
3. extractionthe aqueous layer was extracted with ethyl acetate
4. washThe combined organic phase was washed (3×) with 0.1M HCl
5. dry with materialdried over magnesium sulfate
6. concentrationconcentrated in vacuo
7. customPurification by column chromatography (c-hexane/ethyl acetate, 60/40)