Diethyl Ether → HCID 67085016, compound

Participants

Reaction Conditions

Reaction Steps

The enolate compound of formula (X) obtained in Example 1-1 (33.5 g, 45.1 mmol) was dissolved in diethylether (335 ml). Tetrakis(triphenylphosphine)palladium (2.6 g, 2.25 mmol) was added thereto at room temperature and cooled to 0° C. To the resulting mixture, 1 M trimethylsilyl magnesium chloride (90.2 ml, 90.2 mmol) was added and stirred at room temperature for 1 hr. After completion of the reaction, the resulting mixture was cooled to 0° C. The cooled mixture was quenched with saturated sodium bicarbonate (335 ml) and filtered through Celite. The resulting solid was washed with ethyl acetate, dried over anhydrous sodium sulfate, filtered, and condensed under a reduced pressure. The material thus obtained was purified with column chromatography to obtain the title compound (26.99 g, yield: 87.4%).

Provenance & Evidence