反应详情

温度

0 °C

111 (2 g, 12 mmol), 102 (3.7 g, 12 mmol), triphenylphosphine (9.4 g, 36.1 mmol) and DIPEA (6.2 ml, 36.1 mmol) are dissolved in 50 ml of THF and cooled to 0° C. Then 40% ethyl azodicarboxylate solution in THF (15.7 ml, 36.1 mmol) is added dropwise. After completed addition the mixture is stirred for 16 h (TLC control) at rt. Then the mixture is evaporated under reduced pressure. The residue is diluted with ethyl acetate, washed sat. NaHCO3- and NaCl-solution, and dried over Na2SO4. The crude product is purified by Flash-chromatography (ethyl acetate/hexanes (1:9), silicagel).

1. additionaddition the mixture
2. customThen the mixture is evaporated under reduced pressure
3. additionThe residue is diluted with ethyl acetate
4. washwashed sat. NaHCO3- and NaCl-solution
5. dry with materialdried over Na2SO4
6. customThe crude product is purified by Flash-chromatography (ethyl acetate/hexanes (1:9), silicagel)