反应详情

A solution of 3-hydroxy-1-(2,6,6-trimethyl-3-cyclohexen-1-yl)-1-butanone (2.00 g, 84% pure, 8.0 mmol) in pyridine (1.85 g, 23.4 mmol) was treated at 0° C. with ethyl chloroformate (1.24 g, 23.4 mmol). The reaction solution was stirred at room temperature for 36 hours, treated with aqueous 5% HCl and extracted twice with ether, washed with water, saturated aqueous NaHCO3, then with saturated aqueous NaCl, dried over Na2SO4 and concentrated. The oil thus obtained was purified by flash-chromatography (cyclohexane/AcOEt=98:2), using SiO2 (100 g). Yield: 2.06 g (78%).

1. extractionextracted twice with ether
2. washwashed with water, saturated aqueous NaHCO3
3. dry with materialwith saturated aqueous NaCl, dried over Na2SO4
4. concentrationconcentrated
5. customThe oil thus obtained
6. customwas purified by flash-chromatography (cyclohexane/AcOEt=98:2)