Benzoylacetone → HCID 67530918, compound

Participants

Reaction Steps

A 100 ml four-necked flask equipped with a stirrer, a nitrogen/oxygen inlet tube, a reflex condenser, and a thermometer was charged with 4.87 g of benzoylacetone, 6.89 g of methyl acrylate, and 0.15 g of 1,8-diazabicyclo[5.4.0]-7-undecene, and the mixture was refluxed at 60° C. for 8 hours in a nitrogen/oxygen atmosphere. After cooling, about 100 ml of ethyl acetate was added, and 100 ml of a saturated sodium chloride aqueous solution, 100 ml of ion exchanged water, and 2 ml of 1N hydrochloric acid were further added thereto, followed by stirring. The organic layer was separated, washed with water until neutral, concentrated to dryness, and dried in vacuo at 60° C. to give 9.55 g (95%) of a brown liquid. The brown liquid was identified by various analyses to be an isomeric mixture containing comparative compound No. 1 resulting from addition of 1 mol of benzoylacetone to 2 mol of methyl acrylate.

Provenance & Evidence