反应详情

After 22.2 ml of 50% hydroxylamine aqueous solution was added to a solution of 40.0 g of 8-(2-morpholinoethyl)-8-azabicyclo[3.2.1]octan-3-one in 200 ml of ethanol, the mixture was stirred at room temperature for an hour. The solvent was distilled off and toluene was added followed by azeotropic distillation. After the solvent was distilled off, the residue was purified by silica gel column chromatography (chloroform:NH3 -saturated methanol=20:1) to give 32.8 g of 8-(2-morpholinoethyl)-8-azabicyclo[3.2.1]octan-3-one oxime.

1. distillationThe solvent was distilled off
2. additiontoluene was added
3. distillationfollowed by azeotropic distillation
4. distillationAfter the solvent was distilled off
5. customthe residue was purified by silica gel column chromatography (chloroform:NH3 -saturated methanol=20:1)