反应详情

温度

5 °C

A mixture of Example 18B (1.0 equivalent) and triethylamine (2.3 equivalents) in tetrahydrofuran (0.5 M final concentration based on product from Example 18B) was cooled to 5° C. and treated dropwise with methane sulfonyl chloride (2.3 equivalents) maintaining the temperature below 20° C. After the addition was completed, the reaction mixture was warmed up to ambient temperature for 20 minutes and partitioned with water and methylene chloride. The organic layer was washed with 5% aqueous NaCl solution, dried (Na2SO4), filtered and concentrated. The resulting solid was triturated with isopropyl acetate/heptane (2:1), and the solid was collected by filtration and dried to constant mass (80% yield).

1. temperaturemaintaining the temperature below 20° C
2. additionAfter the addition
3. temperaturethe reaction mixture was warmed up to ambient temperature for 20 minutes
4. custompartitioned with water and methylene chloride
5. washThe organic layer was washed with 5% aqueous NaCl solution
6. dry with materialdried (Na2SO4)
7. filtrationfiltered
8. concentrationconcentrated
9. customThe resulting solid was triturated with isopropyl acetate/heptane (2:1)
10. filtrationthe solid was collected by filtration
11. customdried to constant mass (80% yield)