反应详情

温度

50 °C

3 g (8.4 mmol) of ethyl [2-(2-isobutoxy-5-methoxyphenyl)-2-oxoethyl]-phosphonate dissolved in 20 ml of tetrahydrofuran are added dropwise to a suspension of 1.41 g (12.6 mmol) of potassium tert-butoxide in 30 ml of tetrahydrofuran, heated to 50° C. Heating is continued for 20 minutes at 50° C., the mixture is then cooled to 0° C. and 1.8 g (12.6 mmol) of ethyl 3-methyl-4-oxocrotonate dissolved in 20 ml of tetrahydrofuran are added dropwise. The reaction mixture is then stirred for 72 hours at 25° C. Water is added and the resulting mixture is extracted with ether. After drying (Na2SO4), the solvent is evaporated off and the residue is purified by flash chromatography (dichloromethane) (2.58 g of yellow oil; 89%).

1. temperatureHeating
2. temperaturethe mixture is then cooled to 0° C.
3. additionare added dropwise
4. extractionthe resulting mixture is extracted with ether
5. dry with materialAfter drying (Na2SO4)
6. customthe solvent is evaporated off
7. customthe residue is purified by flash chromatography (dichloromethane) (2.58 g of yellow oil; 89%)