反应详情

温度

15 °C

9.3 g (42.3 mmol) N-(4-hydroxy-butyl)-3-pyridin-3-yl-acrylamide, 11.1 g (42.3 mmol) triphenylphosphine and 8.0 g (42.3 mmol) 4-phenyl-piperidin-2,6-dione are suspended in 120 ml THF, thereafter 6.7 ml (42.3 mmol) azodicarboxylic acid diethyl ester dissolved in 60 ml THF are added dropwise within three hours under protective atmosphere and light cooling (to ca. 15° C.). The mixture is left standing overnight without further cooling at RT. Subsequently, the solvent is removed under vacuum and the residue is chromatographically purified over silica gel with CHCl3/CH3OH (95/5) and, after withdraw of the solvent, crystallized from acetic acid ethyl ester: Colorless crystals with MP. 160–161° C.; Yield 3.8 g (23%).

1. additionare added dropwise within three hours under protective atmosphere and light
2. waitThe mixture is left
3. temperaturewithout further cooling at RT
4. customSubsequently, the solvent is removed under vacuum
5. customthe residue is chromatographically purified over silica gel with CHCl3/CH3OH (95/5)
6. customafter withdraw of the solvent
7. customcrystallized from acetic acid ethyl ester
8. customwith MP. 160–161° C.