反应详情

温度

2 °C

A solution of compound 1 (11.50 g, 0.076 mol) in ethanol (90 ml) was added dropwise to a stirred mixture of compound 7 (15.0 g, 0.069 mol) and tetrakis(triphenylphosphine)palladium(O) (2.38 g, 2.06 mmol) in benzene (130 ml) and 2M-sodium carbonate (100 ml) at room temperature under dry nitrogen. The stirred mixture was heated under reflux (90°-95° C.) for 4.5 h (i.e., until glc analysis revealed absence of starting material). The mixture was cooled and stirred for 1 h at room temperature with 30% hydrogen peroxide (2 ml). The mixture was further cooled to 2° C., and the product was filtered off and washed with water. The product was dried (CaCl2) in vacuo to give fawn-coloured needles.

1. temperatureThe stirred mixture was heated
2. temperatureunder reflux (90°-95° C.) for 4.5 h (i.e., until glc analysis revealed absence of starting material)
3. temperatureThe mixture was cooled
4. filtrationthe product was filtered off
5. washwashed with water
6. dry with materialThe product was dried (CaCl2) in vacuo
7. customto give fawn-coloured needles