Sodium Carbonate → HCID 15008310, compound

Participants

Reaction Steps

To a solution of 1-methyl-4-methlenepiperidine maleate (1.8 g, 0.0081 mol) in saturated sodium bicarbonate (50 mL) was added dibromoformaldoxime (4.94 g, 0.0244 mol) portionwise. The reaction was stirred at room temperature for 1.5 hours. Additional sodium carbonate was added and then the reaction mixture was extracted with chloroform. The extract was dried(MgSO4) and the solvent was evaporated. The residue was purified by flash chromatography on silica gel and elution with ammoniated CHCl3 /EtOAc/MeOH (2/2/1) to give an oil (0.67 g) which solidified. The solid was dissolved in ether and filtered from the insolubles. The filtrate was acidified with maleic acid and the precipitated solid was recrystallized from EtoAc/Et2O to give the bromo derivative as the maleate salt, mp. 159°-160.5° C.

Provenance & Evidence