Azobisisobutyronitrile → HCID 70165804, compound

Participants

Reaction Steps

A mixture of the product from Example 6, Step A (2380 mg, 5.73 mmol), NBS (1530 mg, 8.6 mmol), AIBN (94 mg, 0.57 mmol) in CCl4 (50 mL) was heated under reflux for 17 h. The reaction mixture was cooled to room temperature and filtered. The filtrate was concentrated under vacuum and the residue was purified by SiO2-gel chromatography using 30% EtOAc/hexanes to give the desired product (140 mg). API-MS: 492, 494 (M+1). 1H NMR (300 MHz, CDCl3): d 7.8 (d, 1 H), 7.4 (t, 1 H), 7.2 (d, 1 H), 4.5 (s, 2 H), 5.15 (t, 2 H), 4.0 (s, 3 H), 2.6 (m), 1.8-1.0 (m), 1.4 (s, 9 H).

Provenance & Evidence