Ammonium Hydroxide → 3-Sulfamoylbenzoic acid

HRID 331182

反応式

HRID 331182 の反応式
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]

参加物

3

反応物 2

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

生成物 1

HCID 2293523-Sulfamoylbenzoic acid収率 96%

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-8a3c1443b8594f9bbec8683b39b30023
出典データセット
uspto-grants-2014_11
特許番号
US08877757B2

関連ノート

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