反应详情

To the product of Step A EXAMPLE 27 (300 mg) in THF (5.0 mL) was added MeMgBr (0.92 mL, 1.4 M solution in toluene/THF 3:1) at 0° C. The reaction stirred for 5 minutes before adding chloroacetyl chloride (0.08 mL). The reaction stirred about 7 hours and was diluted with EtOAc, washed with 2 M aqueous HCl and brine. The dried solution (Na2SO4) was concentrated and purified via flash chromatography on silica gel gradient eluted with 0-15% EtOAc in hexane affording the title compound. HPLC/MS: 471.9 (M+1), 473.9 (M+3); Rt=4.32 min.

1. stirringThe reaction stirred about 7 hours
2. washwashed with 2 M aqueous HCl and brine
3. concentrationThe dried solution (Na2SO4) was concentrated
4. custompurified via flash chromatography on silica gel gradient
5. washeluted with 0-15% EtOAc in hexane affording the title compound