Azobisisobutyronitrile → HCID 86725338, compound

Participants

Reaction Conditions

Reaction Steps

Into a 100 ml flask containing the product of step (g) (642 mg, 1.24 mmol) dissolved in EtOH (20 ml), TEA (1.7 ml, 12.4 mmol), hypophosphorous acid (2.3 ml, 12.4 mmol), and AIBN (407 mg, 2.48 mmol) were added. The reaction mixture was heated to 90° C. for 30 minutes, and then the volatiles were evaporated in vacuo. The resulting residue was diluted with water (100 ml) and extracted with DCM (3×). The combined DCM extracts were washed with brine, dried over Na2SO4, and solvent evaporated in vacuo to give the crude product. Purification by silica-gel chromatography (gradient elution: 0 to 30% EtOAc in hexanes) gave the sub-title compound as a white solid that was contaminated with AIBN. This material was used as obtained in the next step. MS: ESI (positive): 392, 394 (M+H).

Provenance & Evidence