反应详情

温度

100 °C

A stirred mixture of Intermediate 63 (0.4 g), Intermediate 28 (0.16 g) and potassium carbonate (0.38 g) in 1,3-dimethyl-3,4,5,6-tetrahydro-2(1H)-pyrimidinone (10 ml) was heated at 100° C. under nitrogen for 3 h. A further portion of Intermediate 28 (0.07 g) was added and the mixture stirred at 60° C. for 23 h. The cooled mixture was diluted with water (100 ml) and extracted with ethyl acetate (3×100 ml). The combined organic extracts were washed with water (2×70 ml) and brine (70 ml), dried over magnesium sulphate and concentrated in vacuo. The residue was purified by chromatography on silica gel eluting with methanol followed by mass directed preparative HPLC (Method A) to give the title compound as a yellow foam (0.12 g).

1. extractionextracted with ethyl acetate (3×100 ml)
2. washThe combined organic extracts were washed with water (2×70 ml) and brine (70 ml)
3. dry with materialdried over magnesium sulphate
4. concentrationconcentrated in vacuo
5. customThe residue was purified by chromatography on silica gel eluting with methanol