反应详情

温度

60 °C

In a dried 100 ml 3-neck flask, 15.2 g(0.1 mole) of 4-trifluoromethyl-3-penten-2-one prepared in Example 2, 13 g(0.1 mole)of ethyl acetoacetate and 3.4 g of sodium ethoxide were added to 60 ml of benzene, and stirred for 4 hrs at 60° C. The reaction mixture was cooled to room temperature and water was added. After neutralization using 10N hydrochloric acid solution, the organic layer was extracted, and dried over magnesium sulfate. The residue was distilled under the vacuum pressure of 1 mmHg, to obtain 11.2 g of the title compound as main product(yield: 58.3%) and 4.5 g of 4-ethoxycarbonyl-3,5-dimethyl-5-trifluoromethyl-2-cyclohexen-1-one(A-2) as by-product(yield: 17%).

1. temperatureThe reaction mixture was cooled to room temperature
2. extractionthe organic layer was extracted
3. dry with materialdried over magnesium sulfate
4. distillationThe residue was distilled under the vacuum pressure of 1 mmHg