4-Chlorobenzenesulfonyl chloride → 2-{[(4-Chlorophenyl)sulfonyl]amino}-4,5-dimethoxybenzoic acid

HRID 1249691ノート

反応式

HRID 1249691 の反応式
C(=O)([O-])[O-].[Na+].[Na+].[NH2:7][C:8]1[CH:16]=[C:15]([O:17][CH3:18])[C:14]([O:19][CH3:20])=[CH:13][C:9]=1[C:10]([OH:12])=[O:11].[Cl:21][C:22]1[CH:27]=[CH:26][C:25]([S:28](Cl)(=[O:30])=[O:29])=[CH:24][CH:23]=1>O>[Cl:21][C:22]1[CH:27]=[CH:26][C:25]([S:28]([NH:7][C:8]2[CH:16]=[C:15]([O:17][CH3:18])[C:14]([O:19][CH3:20])=[CH:13][C:9]=2[C:10]([OH:12])=[O:11])(=[O:30])=[O:29])=[CH:24][CH:23]=1

参加物

5

反応物 3

HCID 73984-Chlorobenzenesulfonyl chlorideHCID 10340Sodium CarbonateHCID 797364,5-Dimethoxyanthranilic acid

生成物 1

HCID 12399912-{[(4-Chlorophenyl)sulfonyl]amino}-4,5-dimethoxybenzoic acid

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
60 °C

実験手順

33.71 g (0.32 mol) of sodium carbonate were dissolved in 250 ml of water and warmed to 60° C. 25.00 g (0.13 mol) of 2-amino-4,5-dimethoxy-benzoic acid were introduced into the solution, and to this solution 29.55 g (0.14 mol) of 4-chloro-benzenesulfonyl chloride were added portionwise over 15 min . After cooling the mixture was filtered with suction, the residue was taken up in 1% sodium hydrogencarbonate solution, the solution filtered, and the product precipitated by addition of 1 N hydrochloric acid. 25.90 g (55%) of 2-(4-chloro-phenylsulfonylamino)-4,5-dimethoxy-benzoic acid of melting point (m.p.) 212-214° C. were obtained.

後処理

  1. temperatureAfter cooling the mixture
  2. filtrationwas filtered with suction
  3. filtrationthe solution filtered
  4. customthe product precipitated by addition of 1 N hydrochloric acid
  5. custompoint (m.p.) 212-214° C.
  6. customwere obtained

出典と根拠

ORDレコード
ord-bbd4b069c47041e8b98b2f5448c9f792
出典データセット
uspto-grants-2002_01
特許番号
US06335334B1

反応ノート

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