反应详情

温度

-10 °C

A solution of Part A 3-bromopropyl sulfonyl chloride (1.06 g, 4.8 mmol) in dichloromethane (5 mL) was added dropwise to a cooled (-10° C.) stirred solution of Example 6a, Part B amine (1.05 g, 3.02 mmol) and triethyl amine (1.44 mL, 9.6 mmol) in dichloromethane (15 mL), After a few minutes, a precipitate formed. The suspension was stirred at -10° C. for 2.5 hours, diluted with dichloromethane (35 mL) and washed with 1N HCl solution (2×15 mL). The dichloromethane solution was dried (MgSO4), filtered and the solvent was removed in vacuo. The crude oil was purified on silica gel (Merck, 150 mL) eluting with 50% ethyl acetate in hexane to give title compound as a white foam (1.160 g, 72%).

1. waitAfter a few minutes
2. customa precipitate formed
3. washwashed with 1N HCl solution (2×15 mL)
4. dry with materialThe dichloromethane solution was dried (MgSO4)
5. filtrationfiltered
6. customthe solvent was removed in vacuo
7. customThe crude oil was purified on silica gel (Merck, 150 mL)
8. washeluting with 50% ethyl acetate in hexane