反应详情

At 0° C., 1.14 g of triphenylphosphine and 0.69 ml of diethyl azodicarboxylate were initially charged in 30 ml of tetrahydrofuran, and the mixture was stirred for 15 min. 1.00 g of 4-(5-chlorooxazolo[5,4-d]pyrimidin-2-yl)-2,6-dimethylphenol, 0.61 ml of triethylamine and 0.90 g of benzyl 3-hydroxycyclobutanecarboxylate were then added, and the reaction was stirred under argon, initially at room temperature for 6 h. Another 1.14 g of triphenylphosphine and 0.69 ml of diethyl azodicarboxylate were then added, and the reaction was stirred for 12 h. After another addition of 1.14 g of triphenylphosphine and 0.69 ml of diethyl azodicarboxylate and 2 further hours of reaction time at room temperature, the reaction was concentrated and the resulting residue was purified by flash chromatography (silica gel, heptane/ethyl acetate). This gave 1.45 g (86%) of the title compound.

1. stirringthe reaction was stirred under argon, initially at room temperature for 6 h
2. stirringthe reaction was stirred for 12 h
3. concentrationthe reaction was concentrated
4. customthe resulting residue was purified by flash chromatography (silica gel, heptane/ethyl acetate)