反应详情

温度

60 °C

The ester from the foregoing step (0.03 g, 0.05 mmol) was dissolved in a mixture of dioxane (7 ml)/water (2 ml). Then LiOH (12 mg, 0.5 mmol) was added and the solution heated to 60° C. for 14 h. The reaction mixture was then diluted with AcOEt (20 ml), washed with 2.0N HCl (20 ml), brine (20 ml), dried over Na2SO4 and concentrated in vacuo. The residue was purified by chromatography on silica gel eluting with 20% AcOEt/Hexane and consequently by HPLC (gradient 60-98% CH3CN/0.1% TFA-H20) to afford 1.2 mg of the title compound; m/z (ES+) 586 (MH+); m/z (ES−) 584 (M−H+).

1. washwashed with 2.0N HCl (20 ml), brine (20 ml)
2. dry with materialdried over Na2SO4
3. concentrationconcentrated in vacuo
4. customThe residue was purified by chromatography on silica gel eluting with 20% AcOEt/Hexane and consequently by HPLC (gradient 60-98% CH3CN/0.1% TFA-H20)