Potassium Hydroxide → HCID 12899691, compound

Participants

Reaction Steps

2.0 g of 8-(1-piperazinyl)-6,7-dihydro-1-oxo-1H,5H-benzo[ij]quinolizine-2-carboxylic acid was dissolved in 20 ml of water having dissolved therein 0.8 g of potassium hydroxide and 0.8 g of methanesulfonyl chloride was added dropwise to the solution. The resulting mixture was allowed to stand overnight at the same temperature as above while stirring. The crystals precipitated were separated by filtration and washed with water. The crystals thus-treated were dissolved in 1 N aqueous sodium hydroxide solution and the solution was treated with activated carbon and rendered neutral with a 10% aqueous hydrochloric acid solution to precipitate crystals, which were separated by filtration and washed with water. Recrystallization of the crystals thus-obtained from dimethylformamide gave 1.0 g of 8-(4-methanesulfonyl-1-piperazinyl)-6,7-dihydro-1-oxo-1H,5H-benzo[ij]quinolizine-2-carboxylic acid as white needles having a melting point of not lower than 300° C.

Provenance & Evidence