Methanesulfonyl chloride → HCID 19701055, compound

Participants

Reaction Conditions

Reaction Steps

1.22 g of the above-mentioned compound (1) and 1.01 g of triethylamine were dissolved in 15 ml of dichloromethane. 5 ml of a dichloromethane solution containing 630 mg of methanesulfonyl chloride was then dropped thereon over a period of 10 minutes, at -15° C. After stirring for 30 minutes at the same temperature, 5 ml of a dichloromethane solution containing 1.14 g of N-formylpiperazine was dropped thereon into the first solution, over a period of 10 minutes, followed by stirring for 1 hour at -5° C. The reaction solution was made alkaline by the addition of saturated sodium bicarbonate solution and then was extracted with dichloromethane (10 ml×3). Next, after washing with saturated brine, the reaction solution was dried with anhydrous sodium sulfate. The solvent was then distilled off under reduced pressure to obtain 1.80 g of residue. This was then purified with silica gel column chromatography (elution solvent: ethyl acetate) to obtain 1.68 g of the target compound. Yield: 98%

Provenance & Evidence