Hydrochloric Acid → 2,4-Dichloro-5-[[(2-fluorophenyl)amino]sulfonyl]benzoic acid

HRID 1951516ノート

反応式

HRID 1951516 の反応式
[Cl:1][C:2]1[CH:12]=[C:11]([Cl:13])[C:10]([S:14]([NH:17][C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=2[F:24])(=[O:16])=[O:15])=[CH:9][C:3]=1[C:4]([O:6]CC)=[O:5].C(O)C.[OH-].[Na+].Cl>O>[Cl:1][C:2]1[CH:12]=[C:11]([Cl:13])[C:10]([S:14]([NH:17][C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=2[F:24])(=[O:16])=[O:15])=[CH:9][C:3]=1[C:4]([OH:6])=[O:5]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 702EthanolHCID 14798Sodium HydroxideHCID 66675729HCID 66675729、化合物

生成物 1

HCID 23243772,4-Dichloro-5-[[(2-fluorophenyl)amino]sulfonyl]benzoic acid

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To the product of Step A was added ethanol (8 mL) followed by a solution of NaOH (0.378 g, 9.45 mmol) in water (8 mL). The reaction was stirred at ambient temperature for 45 minutes. To the mixture was added 1 N HCl (23 mL), and the mixture was stirred overnight. The solids were collected by filtration, washed with water (1×5 mL), and dried by vacuum filtration to give 2,4-dichloro-5-{[(2-fluorophenyl)amino]sulfonyl}benzoic acid: 1H NMR (400 MHz, DMSO-d6) δ ppm 13.50 (bs, 1H), 10.30 (bs, 1H), 8.22 (s, 1H), 8.04 (s, 1H), 7.28-7.11 (m, 4H); MS (ESI) m/z 362.3 (M−H)−.

後処理

  1. stirringthe mixture was stirred overnight
  2. filtrationThe solids were collected by filtration
  3. washwashed with water (1×5 mL)
  4. customdried by vacuum filtration

出典と根拠

ORDレコード
ord-6c71f87fd8d942638329e63a388499ef
出典データセット
uspto-grants-2013_03
特許番号
US08404719B2

反応ノート

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