Iodine → N-(4-iodo-1H-pyrazol-5-yl)acetamide

HRID 588558노트

반응식

HRID 588558 반응식
[NH:1]1[C:5]([NH:6][C:7](=[O:9])[CH3:8])=[CH:4][CH:3]=[N:2]1.[I:10](O)(=O)=O.II>C(O)C>[I:10][C:4]1[CH:3]=[N:2][NH:1][C:5]=1[NH:6][C:7](=[O:9])[CH3:8]

참가 물질

5

반응물 3

HCID 807IodineHCID 24345Iodic acidHCID 27775273-Acetylaminopyrazole

생성물 1

HCID 86717260N-(4-iodo-1H-pyrazol-5-yl)acetamide수율 348.6%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
60 °C

실험 절차

A suspension of N-(1H-pyrazol-5-yl)acetamide (60 g, 0.48 mol), iodic acid (21.1 g, 0.12 mol) and iodine (61 g, 0.24 mol) in ethanol (1.6 L) was heated at 60° C. for 1.5 h and cooled to room temperature. The reaction mixture was concentrated in vacuo and partitioned between ethyl acetate and 2 M Na2S2O3 aq. solution. The layers were separated and the aqueous extracted with ethyl acetate. The combined organic layers were dried (MgSO4), filtered and concentrated in vacuo to provide the title compound as a solid (105 g).

후처리

  1. temperaturecooled to room temperature
  2. concentrationThe reaction mixture was concentrated in vacuo
  3. custompartitioned between ethyl acetate and 2 M Na2S2O3 aq. solution
  4. customThe layers were separated
  5. extractionthe aqueous extracted with ethyl acetate
  6. dry with materialThe combined organic layers were dried (MgSO4)
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-ca67f86654f3424a99b8656ef2bc1a16
출처 데이터셋
uspto-grants-2016_01
특허 번호
US09227976B2

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