Hydrochloric Acid → HCID 20226373, compound

Participants

Reaction Steps

10 g of 3-(3-cyano-4-morpholino-benzoyl)-propionic acid are stirred together with 2.98 g of 35% formaldehyde solution and 76.4 ml of 0.5N sodium hydroxide solution for 16 hours at room temperature. The reaction mixture, whilst being cooled with ice-water and stirred, is then rendered acid with concentrated hydrochloric acid, and is stirred for a further 16 hours at room temperature. Ethyl acetate is afterwards added until two clear phases are formed; the aqueous phase is subsequently separated, and extracted with ethyl acetate. The organic phases are washed twice with 2N sodium carbonate solution, with water and with brine; they are then dried over sodium sulfate and concentrated by evaporation. The 4-(3-cyano-4-morpholino-benzoyl)-butyrolactone obtained as an oily residue is used directly in the following stage.

Provenance & Evidence