反应详情

98.15 g (1.00 mole) Cyclohexanone are mixed with 35.4 g (1.05 mole) ethyl phosphonate and mixed at 25° to 30° C. with 66.1 g (1.04 mole) potassium hydroxide powder (content 88%). The reaction mixture is further stirred for 30 minutes and successively mixed with 150 mL dimethyl sulphoxide and 86.0 g (1.41 mole) nitromethane. This solution is added dropwise at 110° to 115° C. over 35 minutes to a suspension of 64.7 g (0.47 mole) potassium carbonate in 470 mL dimethyl sulphoxide. Then stirring is continued for 2 to 3 hours and the reaction mixture is mixed with water and subsequently extracted several times with n-hexane. The combined organic phases are washed with water, dried over anhydrous sodium sulphate and the solvent then distilled off in a vacuum. 191.5 g ethyl 1-nitromethyl-1-cyclohexaneacetate in the form of an oil are obtained (yield 83% of theory). Composition according to HPLC: 88.7% of the product of Step 2 and 6.3% of the product of Step 1.

1. stirringThen stirring
2. waitis continued for 2 to 3 hours
3. washThe combined organic phases are washed with water
4. dry with materialdried over anhydrous sodium sulphate
5. distillationthe solvent then distilled off in a vacuum