Acrylic Acid → HCID 86743376, compound

Participants

Reaction Steps

Into a 500 ml, three necked round-bottom flask equipped with a cold-finger,addition funnel, and mechanical stirrer were charged approximately 230 ml of hexane, 32.35 ml of acrylic acid, and 5 ml of methyl acrylate. The flask was placed in a water bath at 25° C. and purged with nitrogenfor 45 minutes. Next, 1.26 ml of 1,5-hexadiene (HD) was placed in an addition funnel and diluted to 60 ml with hexane which had been stored under nitrogen. The water bath temperature was raised to reflux temperature (65°-70° C.) and 6 ml (10%) of the HD solution was added to the reaction mixture. The reaction was initiated with 1.0 weight % benzoyl peroxide which had been dissolved in 50 ml of hexane. After a white precipitate began forming (about 5 minutes), the remaining HD solution was added incrementally over a 1-hour period. After addition of the HD solution was complete, the reaction was allowed to proceed for 30 minutes. Product was filtered, washed with hexane, dried under vacuum, and ground into a fine white powder.

Provenance & Evidence