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Hydroxyamine hydrochloride → methyl N-[4-hydroxyiminomethyl-2-methylbenzoyl]carbamate

HRID 552668
ノート
印刷プレビュー

反応式

HRID 552668 の反応式
[CH:1]([C:3]1[CH:15]=[CH:14][C:6]([C:7]([NH:9][C:10](=[O:13])[O:11][CH3:12])=[O:8])=[C:5]([CH3:16])[CH:4]=1)=O.Cl.[NH2:18][OH:19]>CO.O>[OH:19][N:18]=[CH:1][C:3]1[CH:15]=[CH:14][C:6]([C:7]([NH:9][C:10](=[O:13])[O:11][CH3:12])=[O:8])=[C:5]([CH3:16])[CH:4]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 443297Hydroxyamine hydrochlorideHCID 86654470methyl N-[4-formyl-2-methyl benzoyl]carbamate

生成物 1

HCID 86654469methyl N-[4-hydroxyiminomethyl-2-methylbenzoyl]carbamate収率 102.8%

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 41 mg of methyl N-[4-formyl-2-methyl benzoyl]carbamate in 4 mL of methanol and 1 mL of water, 15 mg of hydroxylamine 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 to obtain 45 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

出典と根拠

ORDレコード
ord-8dde2ee248754997a59e3df51e9c064e
出典データセット
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07951828B1

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート