Citric Acid → 2-Methyl-benzaldoxime

HRID 975237

反応式

HRID 975237 の反応式
[CH3:1][C:2]1[CH:9]=[CH:8][CH:7]=[CH:6][C:3]=1[CH:4]=O.[Cl-].[OH:11][NH3+:12].[OH-].[Na+].C(O)(=O)CC(CC(O)=O)(C(O)=O)O>O.C(O)C>[CH3:1][C:2]1[CH:9]=[CH:8][CH:7]=[CH:6][C:3]=1[CH:4]=[N:12][OH:11]

参加物

7

反応物 4

HCID 311Citric AcidHCID 107222-MethylbenzaldehydeHCID 14798Sodium HydroxideHCID 21645Hydroxylamine HCl

生成物 1

HCID 1024012-Methyl-benzaldoxime収率 70.7%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒2 回

実験手順

A mixture of 2-methylbenzaldehyde (10.8 g, 90 mmol), hydroxylammonium chloride (9.4 g, 135 mmol), sodium hydroxide (18.0,0.45 mol), ethanol (80 ml) and water (20 ml) was heated at reflux for 1 h. A solution of citric acid (20 g) in water (700 ml) was added and the mixture was left for crystallisation. The precipitate was collected and recrystallised from water to give 8.6 g of 2-methylbenzaldehyde oxime. M.p. 49.0-49.4° C.

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 1 h
  3. waitthe mixture was left for crystallisation
  4. customThe precipitate was collected
  5. customrecrystallised from water

出典と根拠

ORDレコード
ord-4069212b558c4bb4a2e7772af3b8b12c
出典データセット
uspto-grants-1997_03
特許番号
US05608069

関連ノート

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