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Formic Acid → HCID 178469440, 화합물

HRID 2363750
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HRID 2363750 반응식
[NH:1]([C:3](=[NH:18])[C:4]1[CH:5]=[CH:6][C:7]2[N:8]([CH:10]=[C:11]([C:13]([O:15][CH2:16][CH3:17])=[O:14])[N:12]=2)[CH:9]=1)[NH2:2].[CH:19](O)=O>>[NH:2]1[CH:19]=[N:18][C:3]([C:4]2[CH:5]=[CH:6][C:7]3[N:8]([CH:10]=[C:11]([C:13]([O:15][CH2:16][CH3:17])=[O:14])[N:12]=3)[CH:9]=2)=[N:1]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 284Formic AcidHCID 178469445HCID 178469445, 화합물

생성물 1

HCID 178469440HCID 178469440, 화합물

반응 조건

온도
85 °C

실험 절차

A suspension of 580 mg of ethyl 6-[hydrazino(imino)methyl]imidazo[1,2-a]pyridine-2-carboxylate in 6 mL of formic acid is heated for 20 hours at 85° C. The reaction mixture is concentrated to less than 20% of its initial volume and diluted with 20 mL of water. Solid sodium carbonate is added at 0-5° C. to obtain a pH of 8-9. The precipitate is filtered off by suction, and then purified by chromatography on silica, eluting with a mixture of dichloromethane and methanol (98/2) to give 320 mg of ethyl 6-(1H-1,2,4-triazol-3-yl)imidazo[1,2-a]pyridine-2-carboxylate.

후처리

  1. concentrationThe reaction mixture is concentrated to less than 20% of its initial volume
  2. addition
diluted with 20 mL of water
  • additionSolid sodium carbonate is added at 0-5° C.
  • customto obtain a pH of 8-9
  • filtrationThe precipitate is filtered off by suction
  • custompurified by chromatography on silica
  • washeluting with a mixture of dichloromethane and methanol (98/2)
  • 출처 및 근거

    ORD 기록
    ord-f9a73176561c4b3d9fe3e159e711fc3b
    출처 데이터셋
    uspto-grants-2014_04
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US08691990B2

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