反应详情

温度

100 °C

A mixture of Compound 4 (348 mg, 1.5 mmole) and polyphosphoric acid (80%, 17.5 g) was stirred at 100° C. for 1 hour. Water (150 ml) was added to the reaction mixture, followed by the addition of potassium carbonate to adjust the pH to 5. The resulting mixture was saturated with sodium chloride and then extracted with THF (3 times). The organic layers were combined, washed with saturated brine, dried over anhydrous sodium sulfate, and then concentrated under reduced pressure. The residue was fractionated and purified by chromatography on a silica gel column (eluent: 3%-methanol/chloroform), whereby Compound 5 (161 mg) was obtained (yield: 50%).

1. extractionextracted with THF (3 times)
2. washwashed with saturated brine
3. dry with materialdried over anhydrous sodium sulfate
4. concentrationconcentrated under reduced pressure
5. custompurified by chromatography on a silica gel column (eluent: 3%-methanol/chloroform)