Ethanol → 3,4-Dihydroxythiophene-2,5-dicarboxylic acid

HRID 984761

反応式

HRID 984761 の反応式
CCO.[C:4]([C:9]1[S:10][C:11]([C:16]([O:18]CC)=[O:17])=[C:12]([OH:15])[C:13]=1[OH:14])([O:6]CC)=[O:5].[OH-].[Na+]>O>[C:16]([C:11]1[S:10][C:9]([C:4]([OH:6])=[O:5])=[C:13]([OH:14])[C:12]=1[OH:15])([OH:18])=[O:17]

参加物

5

反応物 3

HCID 702Ethanol2 回HCID 14798Sodium HydroxideHCID 2455033,4-Dihydroxy-thiophene-2,5-dicarboxylic acid diethyl ester

生成物 1

HCID 3162693,4-Dihydroxythiophene-2,5-dicarboxylic acid

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

EtOH (30 mL) was added to 2,5-dicarbethoxy-3,4-dihydroxythiophene (1 g). A solution of NaOH (4.0 g) in H2O (20 mL) was added and refluxed under N for 20 h. Upon cooling to ambient temperature the EtOH was removed by distillation and the residue was redissolved in H2O then acidified with 15% HClaq when a white ppt was obtained This product was collected by filtration and washed with cold H2O then crystallized from dilute MeOH to give colorless needles.

後処理

  1. temperaturerefluxed under N for 20 h
  2. customwas removed by distillation
  3. dissolutionthe residue was redissolved in H2O
  4. customwas obtained This product
  5. filtrationwas collected by filtration
  6. washwashed with cold H2O
  7. customthen crystallized from dilute MeOH
  8. customto give colorless needles

出典と根拠

ORDレコード
ord-0e1c8a71196d4753a61e5b592f8c8adb
出典データセット
uspto-grants-2005_03
特許番号
US06869729B1

関連ノート

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