Ethanol → 5-Methyl-2-furohydrazide

HRID 1889027

반응식

HRID 1889027 반응식
[CH3:1][C:2]1OC=[C:4]([C:7]([O:9]C)=O)[CH:3]=1.[OH2:11].[NH2:12][NH2:13].[CH2:14](O)C>>[CH3:14][C:1]1[O:11][C:4]([C:7]([NH:12][NH2:13])=[O:9])=[CH:3][CH:2]=1

참가 물질

4

반응물 3

HCID 702EthanolHCID 24654Hydrazine hydrate (1:1)2회HCID 23661399Methyl 5-methylfuran-3-carboxylate

생성물 1

HCID 41592505-Methyl-2-furohydrazide

실험 절차

To a solution of methyl 5-methyl-3-furancarboxylate (0.314 mL, 2.5 mmol, commercially available from e.g. Sigma-Aldrich, Fluorochem or Alfa Aesar) in ethanol (20 mL) was added hydrazine monohydrate (0.093 mL, 3.00 mmol) and the solution was stirred under argon and reflux for 18 hours. Analysis by LCMS and TLC showed starting material to still be present, thus more hydrazine monohydrate (0.275 mL, 8.75 mmol) was added and the solution was further stirred under argon and reflux for 18 hours. The solvent was then evaporated in vacuo to yield the product in 0.341 g.

후처리

  1. temperaturereflux for 18 hours
  2. additionwas added
  3. stirringthe solution was further stirred under argon
  4. temperaturereflux for 18 hours
  5. customThe solvent was then evaporated in vacuo
  6. customto yield the product in 0.341 g

출처 및 근거

ORD 기록
ord-493fea9f147c41d3a7718f6062e69261
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08501946B2

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