反应详情

Under an argon atmosphere, stirring and cooling with ice, a solution of triethyl 2-phosphonobutyrate (555 mg, 2.20 mmol) in anhydrous tetrahydrofuran (5 mL) was added dropwise to a solution of potassium tert-butoxide (250 mg, 2.23 mmol) in anhydrous tetrahydrofuran (10 mL), and then the mixture was stirred for 20 minutes. Following this, a solution of 4-methoxy-3-[2-[4-(trifluoromethyl)phenyl]ethoxy]benzaldehyde (650 mg, 2.00 mmol) in anhydrous tetrahydrofuran (5 mL) was added dropwise and then the mixture was stirred for 1 hour under cooling with ice and for 4 hours at room temperature. Cooled 0.5 mol/L hydrochloric acid (30 mL) was added to the reaction mixture, which was extracted with ethyl acetate. The organic layer was washed with water and brine, dried over anhydrous sodium sulfate, and then concentrated. The residue was purified by silica gel column chromatography (eluent: n-hexane:ethyl acetate=6:1 v/v) to afford 842 mg (99%) of the title compound as a colorless oily product.

1. temperaturecooling with ice
2. stirringthe mixture was stirred for 20 minutes
3. additionwas added dropwise
4. stirringthe mixture was stirred for 1 hour
5. additionwas added to the reaction mixture, which
6. extractionwas extracted with ethyl acetate
7. washThe organic layer was washed with water and brine
8. dry with materialdried over anhydrous sodium sulfate
9. concentrationconcentrated
10. customThe residue was purified by silica gel column chromatography (eluent: n-hexane:ethyl acetate=6:1 v/v)