反应详情

To a solution of cis/trans-4-hydroxycyclohexane carboxylic acid ethyl ester (2:1) (5.0 g, 29 mmol) and imidazole (4.4 g, 64 mmol) in N,N-dimethylformamide (90 ml) was added trimethylsilyl chloride (4.0 ml, 32 mmol) at 0-5° C. Stirring for 1 h at room temperature was followed by partitioning between tert-butyl methyl ether (300 ml) and water (150 ml). The layers were separated. The organic layer was washed with two 150-ml portions of water and one 50-ml portion of brine, dried over anhydrous sodium sulfate and concentrated in vacuo to give the title compound (6.7 g, 94%) as colorless oil. MS m/e: 245 ([M+H]+).

1. customby partitioning between tert-butyl methyl ether (300 ml) and water (150 ml)
2. customThe layers were separated
3. washThe organic layer was washed with two 150-ml portions of water and one 50-ml portion of brine
4. dry with materialdried over anhydrous sodium sulfate
5. concentrationconcentrated in vacuo