Hydrochloric Acid → Ethyl 5-aminothiophene-2-carboxylate

HRID 850964

反応式

HRID 850964 の反応式
[CH2:1]([O:3][C:4]([C:6]1[S:7][C:8]([N+:11]([O-])=O)=[CH:9][CH:10]=1)=[O:5])[CH3:2].Cl.[Sn].[OH-].[Na+]>C(Cl)Cl>[NH2:11][C:8]1[S:7][C:6]([C:4]([O:3][CH2:1][CH3:2])=[O:5])=[CH:10][CH:9]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 304627Ethyl 5-nitrothiophene-2-carboxylateHCID 5352426Tin atom

生成物 1

HCID 21585769Ethyl 5-aminothiophene-2-carboxylate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of 60.4 g. of ethyl-5-nitro-2-thiophenecarboxylate and 480 ml. of concentrated hydrochloric acid is cooled in an ice-bath to below -5°. To this mixture is added 72 g. of granular tin in small amounts, keeping the temperature near -5°. After stirring for 6 hours, 575 ml. of 10 N sodium hydroxide is added to neutralize the mixture. Methylene chloride and Celite are added and the mixture is filtered. The methylene chloride layer of the filtrate is separated, dried over sodium sulfate, and filtered through Magnesol. Evaporation affords an oil which is distilled to yield the product.

後処理

  1. additionA mixture of 60.4 g
  2. additionTo this mixture is added 72 g
  3. customnear -5°
  4. filtrationthe mixture is filtered
  5. customThe methylene chloride layer of the filtrate is separated
  6. dry with materialdried over sodium sulfate
  7. filtrationfiltered through Magnesol
  8. customEvaporation
  9. customaffords an oil which
  10. distillationis distilled
  11. customto yield the product

出典と根拠

ORDレコード
ord-7258dbe31670400d8f4a7c2bd8507fcb
出典データセット
uspto-grants-1983_05
特許番号
US04382143

関連ノート

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