反应详情

温度

150 °C

A mixture of 1-cyano-1-(3-fluorophenyl)-3-methoxycarbonylcyclohexan-4-one (57, 51 g, 185 mmol), water (54.8 mL) and DMSO (840 mL) was heated and stirred at 150° C. for 3 hours, followed by stirring at room temperature overnight. The reaction mixture was evaporated and purified by chromatography on silica gel. Elution with ethyl acetate/heptane (5%:95% to 30%:70%) gave 28 g of desired material as a solid product. Rt=3.89 min (Method 3). Detected mass: 218.2 (M+H+).

1. temperaturewas heated
2. stirringby stirring at room temperature overnight
3. customThe reaction mixture was evaporated
4. custompurified by chromatography on silica gel
5. washElution with ethyl acetate/heptane (5%:95% to 30%:70%)