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949-30-4

Benzenesulfonyl chloride, 2,4-dichloro-5-nitro- synthesis

2synthesis methods
-

Yield:949-30-4 60%

Reaction Conditions:

at 0 - 130; for 26 h;

Steps:

326.1 EXAMPLE 326; 5-(Aminosulfonyl)-6-chloro-2-ethyl-1-(4-{2-[({[(4-methylphenyl)sulfonyl]amino}carbonyl)amino]ethyl}phenyl)-1H-benzimidazole; Step 1. 2,4-Dichloro-5-nitrobenzenesulfonyl Chloride

2,4-Dichloronitrobenzene (10 g, 52 mmol) was added ClSO3H (8 ml, 120 mmol) dropwise under ice-water bath. The mixture was stirred at 130° C. for 26 h. The mixture was cooled to rt and poured onto ice-water. The resulting precipitates were collected by filtration and dried under reduced pressure to give 9 g (60%) of the title compound as brown solids. [2917] MS (EI) m/z: 290 (M+). 1H-NMR (CDCl3) δ: 8.70 (1H, s), 7.90 (1H, s).

References:

US2003/236260,2003,A1 Location in patent:Page 119