Hydrochloric Acid → Ethyl 5-aminothiophene-2-carboxylate

HRID 850964

반응식

HRID 850964 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

HCID 21585769Ethyl 5-aminothiophene-2-carboxylate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7258dbe31670400d8f4a7c2bd8507fcb
출처 데이터셋
uspto-grants-1983_05
특허 번호
US04382143

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