反应详情

温度

60 °C

1.84 g (9.9 mmol) of 1-bromo-5-chloropentane [CAS Reg. No. 586-78-7] and 6.45 g (19.8 mmol) of anhydrous cesium carbonate are added to a solution of 1.1 g (2.47 mmol) of methyl 4-{(4E)-5-(2-hydroxyphenyl)-3-[4-(methoxycarbonyl)benzyl]pent-4-en-1-yl}benzoate (racemate; Example 18A) in 16.5 ml of dry toluene, and the mixture is then stirred at 60° C. for 18 h. The mixture is then filtered, and the filtrate is evaporated to dryness. The crude product obtained is taken up in ethyl acetate and washed twice with saturated sodium bicarbonate solution, and the organic phase is dried over sodium sulfate and concentrated. The crude product is then purified by flash chromatography on silica gel (mobile phase: dichloromethane). This gives 1.00 g (1.82 mmol, 73.6% of theory) of a colorless oil.

1. filtrationThe mixture is then filtered
2. customthe filtrate is evaporated to dryness