反应详情

To a solution of 3-bromo-5-chloro-2-fluoroaniline (SM-5, step 3, 0.52 g, 2.3 mmol) in pyridine (2.5 mL) cooled in an ice water bath was added propane-1-sulfonyl chloride (0.3 mL, 2.8 mmol). After 4 hours the solution was concentrated and partitioned between EtOAc (75 mL) and aqueous 0.1 M HCl solution (30 mL). The layers were separated and the organic phase was then washed with brine, dried (Na2SO4) and concentrated to give 778 mg of N-(3-bromo-5-chloro-2-fluorophenyl)propane-1-sulfonamide as a yellow solid which was carried forward without further purification: LCMS (m/z) not observed, tR=0.95 minute.

1. concentrationAfter 4 hours the solution was concentrated
2. custompartitioned between EtOAc (75 mL) and aqueous 0.1 M HCl solution (30 mL)
3. customThe layers were separated
4. washthe organic phase was then washed with brine
5. dry with materialdried (Na2SO4)
6. concentrationconcentrated