Benzaldehyde → HCID 3236994, compound

Participants

Reaction Steps

500 g of benzaldehyde and 476 g of diacetylmonoxime were suspended in 1 L of acetic acid and cooled in an ice bath. At internal temperature of 7° C., hydrochloride gas is slowly blown in to be saturated. At room temperature, the mixture was stirred overnight. The reaction mixture was poured into 1.5 kg of ice, and neutralized with 25% sodium hydroxide solution. The crystalline precipitate was isolated by filtration and washed with 1 L of water and 1 L of diisopropylether. The obtained crystals were dissolved in 3 L of chloroform and insoluble matter was filtered off. The filtrate was dried with 200 g of anhydrous sodium sulfate, filtered, and the filtrate was concentrated in vacuo. 3 L of IPE was added to the residue to be crystallized, the crystal was isolated by filtration, dried under reduced pressure at 50° C. for 1 hour, and 440 g of the subject compound was prepared.

Provenance & Evidence