反应详情

To a magnetically stirred solution of 0.300 g (0.63 mmol) of the product of Example 17 in 6 mL of CH2Cl2 at 0° C. was added 70 μL (0.63 mmol) of 4-chlorobutyryl chloride and 96 mg (0.95 mmol) of triethylamine. The reaction was stirred for 1.5 h and allowed to warm to room temperature. The reaction mixture was then partitioned between saturated aqueous NaHCO3 and EtOAc. The organic layer was separated, washed with aq. NaHCO3, brine, then dried (Na2SO4), filtered and evaporated. The residue was purified on a silica gel flash chromatography column eluted with 0–20% EtOAc-hexane. Evaporation of the purified fractions and drying in vacuo afforded the title compound. HPLC/MS: 577.0 (M+1), 578.9 (M+3); Rt=5.05 min.

1. customThe reaction mixture was then partitioned between saturated aqueous NaHCO3 and EtOAc
2. customThe organic layer was separated
3. washwashed with aq. NaHCO3, brine
4. dry with materialdried (Na2SO4)
5. filtrationfiltered
6. customevaporated
7. customThe residue was purified on a silica gel flash chromatography column
8. washeluted with 0–20% EtOAc-hexane
9. customEvaporation of the purified fractions
10. customdrying in vacuo