反应详情

温度

40 °C

Chloro(1,1-dimethylethyl)dimethylsilane (115 g; 0.76 mol) was added in portions over 1 hour to a solution of commercially available ethyl 4-hydroxycyclohexanecarboxylate (118 g; 0.68 mol), imidazole (103 g; 1.52 mol) and dimethylformamide (400 mL) stirred under an atmosphere of argon. A small exotherm was observed resulting in the reaction mixture temperature increasing to ˜40° C. The mixture was stirred at room temperature overnight then poured into 10% citric acid solution (2 L) and extracted with diethyl ether (2×800 mL). The ether extracts were washed with water, brine and then dried (Na2SO4) and the solvent was removed to give the title compound as an oil (198.4 g)

1. customA small exotherm was observed resulting in the reaction mixture temperature
2. stirringThe mixture was stirred at room temperature overnight
3. extractionextracted with diethyl ether (2×800 mL)
4. washThe ether extracts were washed with water, brine
5. dry with materialdried (Na2SO4)
6. customthe solvent was removed