Potassium Carbonate → HCID 86641475, compound

Participants

Reaction Steps

A mixture of compound 1,2-bis-bromomethyl-3,4-difluoro-benzene (8 g, 0.027 mol), ethyl isocyanoacetate (3.01 g, 0.0266 mol), K2CO3 (22.07 g, 0.159 mol) and tetrabutylammonium hydrogen sulphate (5.45 g, 0.016 mol) in ACN (200 ml) is refluxed for overnight. After complete consumption of starting material the reaction mixture is cooled to RT and ACN is removed under reduced pressure. Water (300 mL) is added to the crude mass and then extracted with EtOAc (3×250 mL). The combined organic extracts are washed with water, dried and concentrated to give a crude product. The crude product is purified by column chromatography (silica, 3% EtOAc in hexane) and the solvent removed to give a viscous liquid (1.6 g, 23.7%).

Provenance & Evidence