反应详情

温度

54 °C

1-(2-Ethyl-butyl)-cyclohexanecarboxylic acid ethyl ester (2.0 g, 8.32 mmol) was added dropwise under stirring to a solution of KOtBu (3.735 g, 33.3 mmol) in THF (15 mL) containing a small amount of water (225 mg, 12.5 mmol). The mixture was stirred 20 h at 54° C., cooled to room temperature, slowly poured onto a mixture of ice and 4N H2SO4 and extracted with DCM (2×150 mL) after adjusting to pH 1. The organic phases were washed with diluted aq. NaCl (100 mL), combined, dried over sodium sulfate and concentrated to afford 1.748 g (99%) 1-(2-ethyl-butyl)-cyclohexanecarboxylic acid, purity 95.2% (GC with internal standard).

1. temperaturecooled to room temperature
2. extractionextracted with DCM (2×150 mL)
3. washThe organic phases were washed with diluted aq. NaCl (100 mL)
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated