Carbon Dioxide → HCID 58232275, compound

Participants

Reaction Conditions

Reaction Steps

250 ml of THF are slowly added to 10.13 g (267.3 mmol) of lithium aluminium hydride, then 71.5 g (190.9 mmol) of 1,2-dicarboxymethyl-3,6-di-o-tolylbenzene, dissolved in 450 ml of THF, are slowly added at such a rate that the temperature does not rise above 40° C. If necessary, the mixture is cooled using dry ice. When the addition is complete, the suspension is heated under reflux for 2 h. When the conversion is complete, a mixture of 120 ml of ethyl acetate and 340 ml of THF is slowly added with cooling at 0° C. (reaction of the excess lithium aluminium hydride with ethyl acetate). When quenching is complete, 300 ml of ethanol are carefully added, and the mixture is subjected to aqueous work-up. 200 ml of water are added, the precipitate is filtered off with suction, and the mother liquor is evaporated a little, extracted with ethyl acetate and dichloromethane, dried over MgSO4 and evaporated, giving 61 g of crude product, which can be employed directly in the next transformation.

Provenance & Evidence