Hydrochloric Acid → 5-Chloro-3-(3,5-dimethylphenylsulfonyl)indole-2-carboxylic acid

HRID 50035ノート

反応式

HRID 50035 の反応式
[OH2:1].[OH-:2].[Li+].[Cl:4][C:5]1[CH:6]=[C:7]2[C:11](=[CH:12][CH:13]=1)[NH:10][C:9]([C:14]([O:16]C)=[O:15])=[C:8]2[S:18][C:19]1[CH:24]=[C:23]([CH3:25])[CH:22]=[C:21]([CH3:26])[CH:20]=1.Cl>O1CCCC1.O>[Cl:4][C:5]1[CH:6]=[C:7]2[C:11](=[CH:12][CH:13]=1)[NH:10][C:9]([C:14]([OH:16])=[O:15])=[C:8]2[S:18]([C:19]1[CH:24]=[C:23]([CH3:25])[CH:22]=[C:21]([CH3:26])[CH:20]=1)(=[O:2])=[O:1]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 168937Lithium hydroxide, monohydrateHCID 11727682Methyl 5-chloro-3-(3,5-dimethylphenylthio)indole-2-carboxylate

生成物 1

HCID 113719555-Chloro-3-(3,5-dimethylphenylsulfonyl)indole-2-carboxylic acid

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 8028Tetrahydrofuran溶媒

実験手順

Lithium hydroxide monohydrate (0.33 g, 0.0079 mol) was added to a solution of methyl 5-chloro-3-(3,5-dimethylphenylthio)indole-2-carboxylate (1.0 g, 0.0026 mol) in tetrahydrofuran (30 mL) and water (30 mL), then reaction was stirred at room temperature for 4 days. After dilution with water the mixture was acidified with 1N HCl and extracted with ethyl acetate. Organic reaction was washed with brine and dried. Evaporation of the solvent furnished 0.94 (100%) of title compound, mp 277-278° C. (from ethanol).

後処理

  1. customreaction
  2. extractionextracted with ethyl acetate
  3. customOrganic reaction
  4. washwas washed with brine
  5. customdried
  6. customEvaporation of the solvent

出典と根拠

ORDレコード
ord-151f78a6f9304158948cef2c4903e3d9
出典データセット
uspto-grants-2004_03
特許番号
US06710068B2

反応ノート

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