Ethanol → 5-Methyl-2-furohydrazide

HRID 1889027

反応式

HRID 1889027 の反応式
[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

参加物

4

反応物 3

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

生成物 1

HCID 41592505-Methyl-2-furohydrazide

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-493fea9f147c41d3a7718f6062e69261
出典データセット
uspto-grants-2013_08
特許番号
US08501946B2

関連ノート

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