Azobisisobutyronitrile → HCID 19365541, compound

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Reaction Steps

The compound (980 mg, 2 mmol) obtained in Example 17, N-bromosuccinimide (NBS) (0.36 g, 2.04 mmol) and α,α-azobisisobutyronitrile (AIBN) (60 mg, 0.37 mmol) were suspended in carbon tetrachloride (250 ml).The mixture was refluxed under heating for 3 hours. After cooling, the reaction mixture was partitioned between chloroform (300 ml) and an aqueous sodium bicarbonate solution. The aqueous layer was extracted with chloroform (100 ml), the extracts were combined, washed with an aqueous sodium chloride solution, dried with Na2SO4, and the solvent was distilled off. Thus obtained residue was recrystallized from dichloromethane-n-hexane to give yellow crystals (1.09 g, 96%).

Provenance & Evidence