1,2-Dichloroethane → HCID 178420050, compound

Participants

Reaction Steps

To a solution of 3-4 (0.2 g, 0.5 mmol), 1H-imidazole-4-carboxylic acid (0.06 g, 0.5 mmol), HOBT (0.06 g, 0.5 mmol), and DIEA (0.2 ml, 1.4 mmol) in DMF (2 ml) was added EDC (0.1 g, 0.6 mmol). The solution was stirred at room temperature for 45 min and was then heated at 80° C. in the microwave for 15 min. The solvent was removed in vacuo. The residue was taken up in DMF (0.5 ml) and was treated with glacial AcOH (2.0 ml). The reaction mixture was heated at 80° C. for 45 min. The reaction was then quenched with water (10 ml) and extracted into EtOAc (3×20 ml). The combined organic layers were concentrated in vacuo to give 22-1 as a brown residue.

Provenance & Evidence