Bromine → HCID 135730604, compound

Participants

Reaction Steps

A mixture of the title compound of Example 52 (6.9 g, 21.8 mmol), bromine (1.35 mL, 26.2 mmol), and sodium acetate (2.7 g, 32.7 mmol) in acetic acid (100 mL) was heated under reflux for 7 h, then allowed to cool. Additional bromine (0.35 mL, 6.8 mmol) was added and the reaction stirred at room temperature for a further 18 h. The reaction mixture was concentrated under reduced pressure and azeotroped with toluene. The residue was partitioned between dichloromethane and water and the resulting precipitate filtered off, washed with dichloromethane, water, then diethyl ether and dried.

Provenance & Evidence