Hydroxyamine hydrochloride → 3-Chloro-4-methylbenzaldoxime

HRID 551311ノート

反応式

HRID 551311 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][C:9]=1[CH3:10])[CH:5]=O.Cl.[NH2:12][OH:13]>CO.O.C(OCC)(=O)C>[Cl:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][C:9]=1[CH3:10])[CH:5]=[N:12][OH:13]

参加物

6

反応物 2

HCID 443297Hydroxyamine hydrochlorideHCID 124230853-Chloro-4-methylbenzaldehyde

生成物 1

HCID 730143123-Chloro-4-methylbenzaldoxime収率 93%

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒

実験手順

In a solution of 5.0 g of 3-chloro-4-methylbenzaldehyde in 40 mL of methanol and 30 mL of water, 4.7 g of hydroxylamine hydrochloride was added, and stirred at room temperature for 2 hours. After the completion of the reaction, the reaction mixture was diluted with 70 mL of ethyl acetate, washed with water (30 mL×1), and then dehydrated with and dried over saturated sodium chloride and anhydrous sodium sulfate in that order, and the solvent was distilled off under reduced pressure to obtain 5.1 g of the aimed product as white crystal. The resulting product was used as such without purification for the next step.

後処理

  1. customAfter the completion of the reaction
  2. washwashed with water (30 mL×1)
  3. dry with materialdried over saturated sodium chloride and anhydrous sodium sulfate in that order
  4. distillationthe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-19a8d61fd57741d48bda3dd5ec5f07cf
出典データセット
uspto-grants-2011_05
特許番号
US07947715B2

反応ノート

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