Hydrochloric Acid → HCID 59331084, compound

Participants

Reaction Steps

A one liter four-necked flask equipped with a stirrer, a nitrogen inlet tube, a reflex condenser, and a thermometer was charged with 35.54 g of 1-[9-ethyl-6-(2-methylbenzoyl)-9H-carbazol-3-yl]ethanone, 264.33 g of ethyl acetate, and 33.66 g of potassium t-butoxide, and the mixture was refluxed in a nitrogen atmosphere for 5 hours. After cooling to room temperature, 100 ml of ion exchanged water and 100 ml of 6N hydrochloric acid were successively added, followed by stirring. The organic phase was separated and washed with a sodium chloride aqueous solution until neutral. A hundred fifty milliliters of n-hexane was added thereto, followed by cooling with ice for crystallization. The solid precipitated was collected by filtration by suction and dried under reduced pressure to give 17.29 g (43%) of pale yellow crystals, which had a melting point of 148° C. and was identified by various analyses to be β-diketone compound No. 3 having a carbazolyl group.

Provenance & Evidence