反应详情

1.6 g of triphenylphosphine and 1 g of 4-Bromo-3-hydroxy-benzoic acid methyl ester were dissolved in 15 ml of anhydrous THF. The solution was cooled to 0° C. to 10° C. and a solution of 0.88 ml DEAD in 5 ml anhydrous THF was added dropwise over 20 min. The reaction was warmed to RT and stirred for 45 min. A solution of 0.69 ml 2-(2,4-Dichlorophenyl)-ethanol in 2 ml anhydrous THF was added with cooling. The reaction was stirred at RT for 3 h, then the solvents were removed under reduced pressure. The residue was treated with n-heptane:ethyl acetate/1:1. The filtrate was dried under reduced pressure. The product was purified by silica gel chromatography, eluting with n-heptane:ethyl acetate/4:1 to n-heptane:ethyl acetate/1:1. Yield 2 g.

1. temperatureThe solution was cooled to 0° C. to 10° C.
2. temperaturewith cooling
3. stirringThe reaction was stirred at RT for 3 h
4. customthe solvents were removed under reduced pressure
5. additionThe residue was treated with n-heptane
6. customThe filtrate was dried under reduced pressure
7. customThe product was purified by silica gel chromatography
8. washeluting with n-heptane