Sodium Hydroxide → HCID 20164602, compound

Participants

Reaction Steps

48 ml of 2 N aqueous sodium hydroxide solution was added over 15 minutes to a stirred, refluxing mixture of 22.5 g of 53A in 48 ml of ethanol. A further 192 ml of 1 N aqueous sodium hydroxide solution was added over 20 minutes to the gently refluxing mixture. Then the mixture was filtered through Celite, and the filtrate was poured into a stirred mixture of 30 ml of concentrated hydrochloric acid, 90 ml of water and about 100 g of ice. The mixture was filtered. The solid was washed with water, dried under reduced pressure, and dissolved in methylene chloride. The solution was dried (MgSO4), filtered and stripped of solvent under reduced pressure. The residue was recrystallized from ethanol/water, and dissolved in methylene chloride. The solution was dried (MgSO4) and the solvent was evaporated to give ((2-ethylphenyl)hydrazono)malonic acid (53B), as a solid, m.p.: 135°-136° C. (with decomposition).

Provenance & Evidence