反应详情

温度

0 °C

To a suspension of sodium hydride (0.004 g; 60% dispersion; 0.111 mmol) in THF (0.5 mL) at 0° C. was added a solution of 0.050 g 0.101 mmol) of the product from Example 26 (in THF (0.5 mL) and the reaction mixture was stirred at 0° C. for 30 minutes. Dimethylsulfamoyl chloride (9 μL; 0.101 mmol) was added dropwise and the reaction was then stirred at room temperature for an additional 5 hours. The reaction was quenched with saturated NaHCO3 solution. The reaction mixture was partitioned between ethyl acetate and saturated NaHCO3 solution. The organic layer was washed twice with saturated NaHCO3 solution, brine, dried (Na2SO4), filtered, and concentrated in vacuo. Purification by MPLC (silica gel; 0% to 50% ethyl acetate:hexane gradient) gave the title compound. HPLC/MS: 564.9 (M+1), 566.9 (M+3); Rt=4.33 min.

1. stirringthe reaction was then stirred at room temperature for an additional 5 hours
2. customThe reaction was quenched with saturated NaHCO3 solution
3. customThe reaction mixture was partitioned between ethyl acetate and saturated NaHCO3 solution
4. washThe organic layer was washed twice with saturated NaHCO3 solution, brine
5. dry with materialdried (Na2SO4)
6. filtrationfiltered
7. concentrationconcentrated in vacuo
8. customPurification by MPLC (silica gel; 0% to 50% ethyl acetate:hexane gradient)