反应详情

Compound (c) and (1,2-diethoxy-2-oxoethyl)(triphenyl)phosphonium chloride (2.89 g, 6.74 mmole) were dissolved in isopropanol (100 ml) and anhydrous potassium carbonate (1.24 g, 9.00 mmole) was added and the mixture was refluxed overnight. The precipitate was filtered off and the solvent evaporated in vacuo. Purification of the crude product with preparative HPLC (Kromasil C8, 10 μm, 50×500 mm) using acetronitrile (50-70%) in ammonium acetate buffer (pH 7) as mobile phase gave 0.88 g (46% yield) of the desired product.

1. temperaturethe mixture was refluxed overnight
2. filtrationThe precipitate was filtered off
3. customthe solvent evaporated in vacuo
4. customPurification of the crude product with preparative HPLC (Kromasil C8, 10 μm, 50×500 mm)