反应详情

A solution of sodium tert-pentoxide (70 ml of a 1M solution), prepared for immediate use, is added to a suspension of methyl(triphenyl)phosphonium iodide (25 g, 61.8 mmol) in 50 ml of toluene, and the mixture is stirred at room temperature under nitrogen for 20 minutes. The compound obtained in Step 1 (6.70 g, 20.6 mmol) dissolved in 50 ml of toluene is added dropwise and the reaction mixture is refluxed for 3 hours. After cooling, the reaction mixture is hydrolysed with a saturated NH4Cl solution and extracted with ether. The organic phase is washed with a saturated NaCl solution, H2O, dried over MgSO4 and concentrated in vacuo. The title product is purified by flash chromatography over a column (SiO2, toluene/cyclohexane:60/40).

1. additionis added dropwise
2. temperaturethe reaction mixture is refluxed for 3 hours
3. temperatureAfter cooling
4. extractionextracted with ether
5. washThe organic phase is washed with a saturated NaCl solution, H2O
6. dry with materialdried over MgSO4
7. concentrationconcentrated in vacuo
8. customThe title product is purified by flash chromatography over a column (SiO2, toluene/cyclohexane:60/40)