反应详情

温度

0 °C

100 (4 g, 21.9 mmol), 102 (6.7 g, 21.9 mmol), triphenylphosphine (17.3 g, 65.8 mmol) and 40% diethyl azadicarboxylate solution (31.8 ml, 65.8 mmol) are dissolved in THF and cooled to 0° C. Then a solution of N-ethyldiisopropylamine (11.2 ml, 65.8 mmol) in THF is added dropwise. After the addition is completed, the mixture is stirred at room temperature for 2 h. Then the mixture is evaporated under reduced pressure. The residue is diluted with ethyl acetate, washed with saturated NaHCO3-solution and dried over Na2SO4. The crude product is purified by Flash-chromatography (ethyl acetate/hexanes (3:7), silicagel).

1. additionAfter the addition
2. customThen the mixture is evaporated under reduced pressure
3. additionThe residue is diluted with ethyl acetate
4. washwashed with saturated NaHCO3-solution
5. dry with materialdried over Na2SO4
6. customThe crude product is purified by Flash-chromatography (ethyl acetate/hexanes (3:7), silicagel)