Acetanilide → HCID 131714647, compound

Participants

Reaction Steps

5 Grams of o-methoxycarbonyl- -[4-3,4-dimethoxybenzoyl)-1-piperazinyl]acetanilide was suspended in 50 ml of dimethylformamide, then 621 mg of 50% oily sodium hydride was added to the suspension and stirred at a room temperature for 1 hour. Next, under ice-cooled condition, 2.5 g of methyl iodide was added dropwise to the suspention and stirred at a room temperature for 4 hours. The solvent was removed by distillation under a reduced pressure, the residue obtained was extracted with chloroform and 1N-sodium hydroxide aqueous solution. The chloroform layer was washed with water, dried and then chloroform was removed by distillation. The residue obtained was purified by a silica gel column chromatography, and the product obtained was converted into an oxalate, recrystallized from methanol-ether to obtain 3.11 g of o-methoxy-carbonyl-N-methyl-α-[4-dimethoxy-benzoyl)-1-piperazinyl]-acetanilide dioxalate in the form of colorless powdery crystals. Melting point: 181.0°-182.0° C. (decomposed).

Provenance & Evidence