反应详情

Ethyl 2-[3-(allyloxycarbonylmethyl)phenoxy]-2-methylpropionate (6.40 g, 20.9 mmol) was dissolved in tetrahydrofuran (150 mL). Subsequently, triphenylphosphine (2.42 g, 2.09 mmol) and piperidine (41.34 mL, 41.8 mmol) were added thereto. Under argon atmosphere, tetrakis(triphenylphosphine)palladium (2.42 g, 2.09 mmol) was added, the resultant mixture was stirred for three hours at room temperature. After completion of reaction, the reaction mixture was concentrated under reduced pressure, followed by addition of chloroform and washing sequentially with 3M hydrochloric acid, water, and saturated brine. The resultant mixture was subjected to drying over sodium sulfate, concentration under reduced pressure, and purification by silica gel column chromatography (chloroform/methanol/acetic acid=50/1/0.5), whereby the target compound was obtained (6.88 g, 25.84 mmol, >q.).

1. customAfter completion of reaction
2. concentrationthe reaction mixture was concentrated under reduced pressure
3. additionfollowed by addition of chloroform
4. washwashing sequentially with 3M hydrochloric acid, water, and saturated brine
5. dry with materialto drying over sodium sulfate, concentration under reduced pressure, and purification by silica gel column chromatography (chloroform/methanol/acetic acid=50/1/0.5), whereby the target compound
6. customwas obtained (6.88 g, 25.84 mmol, >q.)