4-Bromo-2-chlorobenzenesulfonyl chloride → HCID 58988150, compound

Participants

Reaction Steps

6-[cis-3,5-dimethyl-1-piperazinyl]-3-(methyloxy)-2-pyridinamine (D7, Method C) (473 mg, 2 mmol) was dissolved in pyridine (5 ml) and dichloromethane (5 ml). 4-Bromo-2-chlorobenzene sulfonyl chloride (870 mg, 3 mmol) was added and the solution stirred at room temperature for 5 hours. The mixture was concentrated in vacuo and azeotroped with methanol. The residue was loaded on to an SCX cartridge (Varian, 10 g) in methanol, washed with methanol and the basic products eluted with 2M ammonia/methanol. The product containing fractions were concentrated in vacuo and purified by flash chromatography (Biotage SP4, 40+S, 0-20% 2M ammonia/methanol in dichloromethane to afford the title product (D11), 478 mg, MS (ES+) m/e 489/491/493 [M+H]+.

Provenance & Evidence