Hydroxyamine hydrochloride → HCID 136335088、化合物

HRID 268597ノート

反応式

HRID 268597 の反応式
[CH2:1]([N:3]1[C:7]([CH:8]=O)=[N:6][CH:5]=[N:4]1)[CH3:2].Cl.[NH2:11][OH:12].C(=O)(O)[O-].[Na+]>C(O)C>[CH2:1]([N:3]1[C:7]([CH:8]=[N:11][OH:12])=[N:6][CH:5]=[N:4]1)[CH3:2]

参加物

5

反応物 3

HCID 443297Hydroxyamine hydrochlorideHCID 516892Sodium BicarbonateHCID 280649451-ethyl-1H-1,2,4-triazole-5-carbaldehyde

生成物 1

HCID 136335088HCID 136335088、化合物収率 31.1%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of crude 1-ethyl-1H-1,2,4-triazole-5-carbaldehyde (17.7 g), hydroxylamine hydrochloride (12.7 g, 0.182 mol), sodium bicarbonate (15.3 g, 0.182 mol) and ethanol (60 mL) was heated at reflux for 3 hours. After cooling, the reaction was filtered and the filtrate concentrated in vacuo. The resulting residue was crystallised from ethanol to give the title compound (6.17 g) 1H-NMR (d6-DMSO) δ 1.32 (3H, t, J=7 Hz), 4.41 (2H, q, J=7 Hz), 8.02 (1H, s), 8.25 (1H, s), 12.70 (1H, s)

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 3 hours
  3. temperatureAfter cooling
  4. filtrationthe reaction was filtered
  5. concentrationthe filtrate concentrated in vacuo
  6. customThe resulting residue was crystallised from ethanol

出典と根拠

ORDレコード
ord-7571bf433bdc40b49aa7e5a7ec38dfd3
出典データセット
uspto-grants-2008_11
特許番号
US07446117B2

反応ノート

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