反应详情

A mixture of ethyl (RS)-2-[2-(1,1-dimethylethyl)pyrimidin-5-yl]-3,3-dimethylbutanoate (0.07 g), 2,3,5,6-tetrafluoro-4-methylbenzyl alcohol (0.1 g), titanium IV ethoxide (catalytic amount) and dry toluene (2 cm3) was heated at the reflux temperature for 10 hours. After cooling, the solvent was evaporated under reduced pressure to leave a brown gum, which was purified by preparative thin layer chromatography on 20 cm×20 cm×0.2 cm silica gel plates, eluting with dichloromethane containing 2% by volume ethyl acetate, to give the title compound (0.05 g) as an oil which solidified on standing.

1. temperaturewas heated at the reflux temperature for 10 hours
2. temperatureAfter cooling
3. customthe solvent was evaporated under reduced pressure
4. customto leave a brown gum, which
5. customwas purified by preparative thin layer chromatography on 20 cm×20 cm×0.2 cm silica gel plates
6. washeluting with dichloromethane containing 2% by volume ethyl acetate