反应详情

A solution of the product of Example 157A (1.2 g, 4.4 mmol) and triethylamine (0.49 g, 4.8 mmol) in dichloromethane (25 mL) was treated dropwise with ethyl chloromalonate (0.73 g, 4.8 mmol), stirred for 2 hr and partitioned between ethyl acetate and water and the layers were separated. The ethyl acetate layer was washed with brine, dried (Na2SO4), and concentrated. The residue was purified by column chromatography on silica gel eluting with hexane and ethyl acetate (3:1) to provide the title compound (1.1 g, 65%). MS (DCI) m/z 387 (M+H)+.

1. custompartitioned between ethyl acetate and water
2. customthe layers were separated
3. washThe ethyl acetate layer was washed with brine
4. dry with materialdried (Na2SO4)
5. concentrationconcentrated
6. customThe residue was purified by column chromatography on silica gel eluting with hexane and ethyl acetate (3:1)