Sodium Hydroxide → 2-amino-4,5-dimethylthiophene-3-carboxylic acid

HRID 1973411ノート

反応式

HRID 1973411 の反応式
[NH2:1][C:2]1[S:3][C:4]([CH3:13])=[C:5]([CH3:12])[C:6]=1[C:7]([O:9]CC)=[O:8].[OH-].[Na+]>C(O)C.O.C(O)(=O)C>[NH2:1][C:2]1[S:3][C:4]([CH3:13])=[C:5]([CH3:12])[C:6]=1[C:7]([OH:9])=[O:8]

参加物

6

反応物 2

HCID 14798Sodium HydroxideHCID 78536Ethyl 2-amino-4,5-dimethyl3-thenoate

生成物 1

HCID 37266372-amino-4,5-dimethylthiophene-3-carboxylic acid

試薬・触媒・溶媒 3

HCID 176Acetic Acid溶媒HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

A mixture of 15 parts of ethyl 2-amino-4,5-dimethylthiophene-3-carboxylate and 75 parts by volume of 2N solution of sodium hydroxide in 50% aqueous ethanol is refluxed for 2.5 hours. After cooling the solution is diluted with 75 parts by volume of water and neutralized with acetic acid under cooling with ice. The resulting precipitate is collected by filtration to give 2-amino-4,5-dimethylthiophene-3-carboxylic acid as crystals. Recrystallization from chloroform with charcoal gives colorless needles melting at 136°-138° C (decomposition).

後処理

  1. temperatureis refluxed for 2.5 hours
  2. temperatureAfter cooling the solution
  3. temperatureunder cooling with ice
  4. filtrationThe resulting precipitate is collected by filtration

出典と根拠

ORDレコード
ord-6688fa80f3c548d984986a4d1100f606
出典データセット
uspto-grants-1976_12
特許番号
US03997545

反応ノート

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