Hydroxyamine hydrochloride → HCID 136337818、化合物

HRID 1187996ノート

反応式

HRID 1187996 の反応式
[CH:1]([C:3]1[CH:15]=[CH:14][C:6]([C:7]([NH:9][CH:10]=[N:11][O:12][CH3:13])=[O:8])=[C:5]([CH3:16])[CH:4]=1)=O.Cl.[OH:18][NH2:19]>CO.O>[OH:18][N:19]=[CH:1][C:3]1[CH:15]=[CH:14][C:6]([C:7]([NH:9][CH:10]=[N:11][O:12][CH3:13])=[O:8])=[C:5]([CH3:16])[CH:4]=1

参加物

5

反応物 2

HCID 443297Hydroxyamine hydrochlorideHCID 1363378174-formyl-N-(methoxyiminomethyl)-2-methyl benzoic acid amide

生成物 1

HCID 136337818HCID 136337818、化合物収率 102.4%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒2 回

実験手順

In a solution of 64 mg of 4-formyl-N-(methoxyiminomethyl)-2-methyl benzoic acid amide in 4 mL of methanol and 1 mL of water, 30 mg of hydroxyamine hydrochloride was added at room temperature with stirring, and continued to stir at the same temperature for 1.5 hour. After the completion of the reaction, 10 mL of water was added in the reaction mixture, and extracted with ethyl acetate (10 mL×2). The combined organic phases were dehydrated with and dried over saturated sodium chloride aqueous solution and then anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified with silica gel column chromatography that were eluated with ethyl acetate-hexane (1:1) to obtain 70 mg of the aimed product as white crystal.

後処理

  1. stirringto stir at the same temperature for 1.5 hour
  2. additionwas added in the reaction mixture
  3. extractionextracted with ethyl acetate (10 mL×2)
  4. dry with materialdried over saturated sodium chloride aqueous solution
  5. distillationanhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure
  6. customThe residue was purified with silica gel column chromatography that

出典と根拠

ORDレコード
ord-4f749600d82b4328ba4f0135108c9089
出典データセット
uspto-grants-2014_03
特許番号
US08673951B2

反応ノート

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