Water → HCID 22574217, compound

Participants

Reaction Steps

From 100 ml of ethanol and 1.97 g (0.0855 mol) of sodium, a sodium ethoxide solution is prepared to which 26.6 g (0.0855 mol) of 3,3′-dichlorobenzilic acid in 50 ml of ethanol are added dropwise. The mixture is then stirred for 4 h at ambient temperature. After the solvent has been distilled off the residue is dissolved in 150 ml DMF and 24.27 g (0.171 mol) of methyl iodide are added dropwise, then stirred for another 24 h. While cooling with ice, 300 ml of water and 200 ml of diethylether are added dropwise, the phases are separated, the aqueous phase is extracted with diethylether, then the organic phases are washed with Na2CO3 solution and shaken with water till neutral. After drying over Na2SO4 the mixture is evaporated to dryness. Yield: 22.91 g of yellow oil (=82% of theory).

Provenance & Evidence