反应详情

A solution of the above cyclohexyl-acetaldehyde (1.04 g, 8.25 mmol) and ethyl acetoacetate (0.873 mL, 6.85 mmol) in 300 mL ethanol was stirred in an ice bath as piperidine (7.3 uL, 73 umol) in 380 uL ethanol was added. The mixture was stirred in the ice bath for 5 hours and placed in a refrigerator for 16 hours. The reaction mixture was diluted with 50 mL ether and extracted with saturated sodium chloride (3×30 mL containing 2 drops AcOH). The brine layers were back-extracted with ether (2×40 mL). The combined ether layers were washed with brine (30 mL), dried over sodium sulfate, filtered and evaporated to give 2-acetyl-4-cyclohexyl-but-2-enoic acid ethyl ester (1.79 g).

1. additionwas added
2. extractionextracted with saturated sodium chloride (3×30 mL containing 2 drops AcOH)
3. extractionThe brine layers were back-extracted with ether (2×40 mL)
4. washThe combined ether layers were washed with brine (30 mL)
5. dry with materialdried over sodium sulfate
6. filtrationfiltered
7. customevaporated