Ethyl Acetate → HCID 19907358, compound

Participants

Reaction Steps

First, 525 mg of lithium aluminium hydride was added to 30 ml of absolute tetrahydrofuran, then 20 ml of a solution of 2.39 g 1,4-bis(4,4-diethoxycarbonylbutyl)benzene in absolute tetrahydrofuran was added dropwise thereto with stirring at a room temperature, and the mixture was refluxed for one hour. After adding 4 ml of ethyl acetate with ice-cooling, the reaction mixture was stirred for 10 minutes. To the mixture were further added successively 0.5 ml of water, 0.5 ml of 15% sodium hydroxide aqueous solution and 1.5 ml of water, and the mixture was stirred for one hour. After filtering off insoluble matter, the filtrate was evaporated under a reduced pressure. The oily residue thus obtained was applied to a silica gel column and eluted with chloroform/ethanol (5:1) to obtain 350 mg of the title compound as a colorless crystal.

Provenance & Evidence