4-Chlorobenzenesulfonyl chloride → 5-bromo-N-[2-(4-chlorobenzenesulfonylamino)-4-fluorophenyl]-2-methoxybenzenesulfonamide

To a solution of 5-bromo-N-(4-fluoro-2-aminophenyl)-2-methoxybenzenesulfonamide (0.1 mmol) in pyridine (0.5 mL) and DCM (2 mL), 4-chlorobenzenesulfonyl chloride (0.12 mmol) was added. The reaction mixture was stirred at room temperature for 4 h and then diluted with ethyl acetate (10 mL). The contents were washed with 10% aqueous HCl (10 mL) and brine (10 mL), dried over sodium sulfate, and concentrated under vacuum. The residue obtained was purified by column chromatography eluting with hexanes/ethyl acetate (1:1) followed by ethyl acetate to give 43 mg of 5-bromo-N-[2-(4-chlorobenzenesulfonylamino) -4-fluorophenyl]-2-methoxybenzenesulfonamide. LC: Tr 1.10 min, MS: 551.8 (M+1)+

1. washThe contents were washed with 10% aqueous HCl (10 mL) and brine (10 mL)
2. dry with materialdried over sodium sulfate
3. concentrationconcentrated under vacuum
4. customThe residue obtained
5. customwas purified by column chromatography
6. washeluting with hexanes/ethyl acetate (1:1)

ORD-Eintrag

ord-d8c9d71a0ef041cba4c306be9a74da85

Quelldatensatz

uspto-grants-2009_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07582673B2