Potassium Hydroxide → 5-Nitro-1-benzothiophene-2-carboxylic acid

HRID 1384842

反応式

HRID 1384842 の反応式
C([O:3][C:4]([C:6]1[S:10][C:9]2[CH:11]=[CH:12][C:13]([N+:15]([O-:17])=[O:16])=[CH:14][C:8]=2[CH:7]=1)=[O:5])C.[OH-].[K+]>CCO.O>[N+:15]([C:13]1[CH:12]=[CH:11][C:9]2[S:10][C:6]([C:4]([OH:5])=[O:3])=[CH:7][C:8]=2[CH:14]=1)([O-:17])=[O:16]

参加物

5

反応物 2

HCID 14797Potassium HydroxideHCID 737499Ethyl 5-nitro-1-benzothiophene-2-carboxylate

生成物 1

HCID 2389395-Nitro-1-benzothiophene-2-carboxylic acid収率 85%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

10 g (39.8×10−3 moles) 5-nitrobenzo[b]thiophen-2-carboxylic acid ethyl ester in 250 ml of EtOH and 60 ml of H2O were reacted with 3.8 g (67.8×10−3 moles) of KOH at 60° C. for 2 hours, after which the potassium salt of the product was collected by filtration. A further fraction of the product was collected on adding isopropanol to the filtrate. The salt was dissolved in water and after acidulating the solution with HCl(c), the protonated form of the acid was precipitated out. It was purified by recrystallisation in H2O/EtOH. Yield: 85%.

後処理

  1. filtrationafter which the potassium salt of the product was collected by filtration
  2. customA further fraction of the product was collected
  3. additionon adding isopropanol to the filtrate
  4. dissolutionThe salt was dissolved in water
  5. customthe protonated form of the acid was precipitated out
  6. customIt was purified by recrystallisation in H2O/EtOH

出典と根拠

ORDレコード
ord-2a480e7db0ff45ca8549bc82c30e3218
出典データセット
uspto-grants-2001_07
特許番号
US06262056B1

関連ノート

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