Ammonium Hydroxide → 3-Sulfamoylbenzoic acid

HRID 331182

반응식

HRID 331182 반응식
Cl[S:2]([C:5]1[CH:6]=[C:7]([CH:11]=[CH:12][CH:13]=1)[C:8]([OH:10])=[O:9])(=[O:4])=[O:3].[OH-].[NH4+:15]>>[NH2:15][S:2]([C:5]1[CH:6]=[C:7]([CH:11]=[CH:12][CH:13]=1)[C:8]([OH:10])=[O:9])(=[O:4])=[O:3]

참가 물질

3

반응물 2

HCID 14923Ammonium HydroxideHCID 77641Benzoic acid, 3-(chlorosulfonyl)-

생성물 1

HCID 2293523-Sulfamoylbenzoic acid수율 96%

실험 절차

To ice-cold solution of ammonium hydroxide (25%, 250 ml) is added 3-(chlorosulfonyl)benzoic acid (25 g, commercially available, Aldrich) portionwise and the mixture is stirred at room temperature for 15 h. The solvent is removed under vacuum to about 50 ml and the mixture is acidified with cone. HCl. The precipitate is collected by filtration and dried under vacuum to afford 22 g (96%) of the title compound as a white solid. 1H NMR (DMSO-d6) δ 13.44 (br s, 1H), 8.38 (s, 1H), 8.14 (d, J=7.5 Hz, 1H), 8.04 (d, J=7.9 Hz, 1H), 7.72 (t, J=7.9 Hz, 1H), 7.49 (s, 2H), HPLC (max plot) 97%; Rt 0.68 min. LC/MS: (ES−): 199.8.

후처리

  1. customThe solvent is removed under vacuum to about 50 ml
  2. filtrationThe precipitate is collected by filtration
  3. customdried under vacuum

출처 및 근거

ORD 기록
ord-8a3c1443b8594f9bbec8683b39b30023
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08877757B2

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