反应详情

A mixture of 4-(diethoxyphosphorylmethyl)benzenecarboxylic acid (440 mg) produced according to JP-A 11-60537, potassium tert-butoxide (340 mg) and THF (5.5 mL) was stirred at room temperature for about 1.5 hours, and then a THF solution (1.0 mL) of 2-formylthiazole (200 mg) was dropwise added thereto. After heated overnight under reflux, water was added to the reaction solution, and extracted with ethyl acetate. The organic layer was dried with anhydrous magnesium sulfate, and the solvent was evaporated off under reduced pressure. The resulting residue was purified through silica gel column chromatography (ethyl acetate/methanol=9/1), and the resulting purified product was further purified through reversed-phase HPLC to obtain the entitled compound (7 mg).

1. customproduced
2. temperatureAfter heated overnight
3. temperatureunder reflux
4. extractionextracted with ethyl acetate
5. dry with materialThe organic layer was dried with anhydrous magnesium sulfate
6. customthe solvent was evaporated off under reduced pressure
7. customThe resulting residue was purified through silica gel column chromatography (ethyl acetate/methanol=9/1)
8. customthe resulting purified product
9. customwas further purified through reversed-phase HPLC