2-amino-4-bromobenzene-1-sulfonamide synthesis

Yield:54734-81-5 98%

Reaction Conditions:

with hydrogen iodide in water at 90; for 4 h;

Steps:

5.3 the preparation of compound

5-4 A suspension of compound 5-3 (2.12 g, 7.5 mmol) in HI (25.0 mL, 57% aq.) was stirred at 90 °C for 4.0 hrs. After cooling to rt. the dark purple mixture was diluted with EtOAc (50 mL) and washed successively with saturated aq. Na₂S₂0₃, saturated aq NaHC< and brine. The colorless organic layers were dried over anhydrous Na₂S0₄ and concentrated in vacuo. The crude product was purified by high-performance liquid chromatography (eluent: CH₃CN/H₂0 from 22/78 to 52/48 with 0.01% NH_:,.H₂0 as buffer), resulting in compound 5-4 (1.86 g, 98%). The compound was characterized by the following spectroscopic data: MS (ESI. pos.ion) mlz: 251.5 [M+H] ^" ; and NMR (400 MHz, CDCh) S (ppm): 7.62-7.60 (m, 1H), 7.18-7.15 (m.2H).4.85 (brs.4H).

References:

WO2014/82379,2014,A1 Location in patent:Page/Page column 130; 131; 132