Bromine → HCID 67624138, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of 0.50 g of the title compound of Step A in 200 mL of chloroform was cooled to 0° C. To this mixture was added a solution of 0.45 g of bromine in 35 mL of chloroform dropwise. The mixture was stirred at room temperature for 2 h and then 10% aqueous sodium thiosulfate solution was added. The organic layer was separated and dried over MgSO4, filtered, and concentrated under reduced pressure to dryness. The resulting residue was crystallized from 1-chlorobutane to yield 0.41 g of the title compound of Step B as a solid melting at 145° C. (dec.). 1H NMR (CDCl3): δ 2.49 (s, 3H), 2.56 (s, 3H), 3.11 (br s, 2H), 3.48 (m, 2H), 4.24 (br s, 2H), 7.57 (s, 1H).

Provenance & Evidence