反应详情

温度

120 °C

(1S,4S)-1-(2-Hydroxy-ethyl)-2-oxa-3-aza-bicyclo[2.2.2]oct-5-ene-3-carboxylic acid tert-butyl ester (11) (620 mg, 2.41 mmol) is dissolved in 24 ml of propionitrile and after addition of amine 6 (480 mg, 2.41 mmol), cyanomethyl-trimethyl-phosphonium iodide (796 mg, 6 mmol) and diisopropyl ethyl amine (2 ml, 12 mmol) the mixture is stirred for 16 h at 120° C. Then the mixture is evaporated under reduced pressure. The residue is diluted with ethyl acetate, washed 10% K2CO3- and NaCl-solution, and dried over Na2SO4. The crude product is purified by Flash-chromatography (ethyl acetate/hexanes (9.5:0.5), silicagel).

1. customThen the mixture is evaporated under reduced pressure
2. additionThe residue is diluted with ethyl acetate
3. washwashed 10% K2CO3- and NaCl-solution
4. dry with materialdried over Na2SO4
5. customThe crude product is purified by Flash-chromatography (ethyl acetate/hexanes (9.5:0.5), silicagel)