反应详情

Into a 3 l capacity three-necked flask were added pyridium chlorochromate (161.7 g, 0.75 mol) and dichloromethane(1,000 ml), followed by agitating these, adding a dichloromethane solution (800 ml) of 4-{trans-4'-(hydroxymethyl]cyclohexyl}benzonitrile(107.6 g, 0.5 mol) at 20° C., agitating these for 90 minutes while keeping the temperature at 20° C., adding diethyl ether (1,500 ml), decanting the supernatant, passing the supernatant through a Florisil (trademark of the Floridin Company) column, concentrating under reduced pressure to obtain the captioned compound (101.2 g). Its structure was confirmed according to NMR spectra.

1. stirringagitating these for 90 minutes
2. customat 20° C.
3. customdecanting the supernatant
4. concentrationconcentrating under reduced pressure