Methyl iodide → HCID 67711340, compound

Participants

Reaction Steps

1.04 g of 60% sodium hydride was added to 100 ml of 9.67 g of 3-ethoxycarbonyl-6-isobutyl-1-(2-tetrahydropyranyloxy)piperazine-2,5-dione in anhydrous N,N-dimethylformamide, on ice cooling, and the mixture was stirred for 10 minutes. Thereto was added 3.5 ml of methyl iodide. The mixture was stirred at room temperature for 5 hours. The reaction mixture was ice-cooled and poured into an aqueous solution saturated with ammonium chloride. The mixture was extracted with ethyl acetate. The extract was washed three times with an aqueous solution saturated with sodium chloride, dried with anhydrous magnesium sulfate, and subjected to distillation to remove the solvent to obtain 8.53 g of (3RS,6SR)-3-ethoxycarbonyl-6-isobutyl-3-methyl-1-(2-tetrahydropyranyloxy)piperazine-2,5-dione as a brown oily substance.

Provenance & Evidence