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Water → methyl N-[2-chloro-5-(1-hydroxyiminoethyl)benzyl]carbamate

HRID 2414254
ノート
印刷プレビュー

反応式

HRID 2414254 の反応式
[Cl:1][C:2]1[CH:13]=[CH:12][C:11]([C:14](=O)[CH3:15])=[CH:10][C:3]=1[CH2:4][NH:5][C:6](=[O:9])[O:7][CH3:8].Cl.[NH2:18][OH:19].C([O-])(=O)C.[Na+].O>C(O)C.C(OCC)(=O)C>[Cl:1][C:2]1[CH:13]=[CH:12][C:11]([C:14](=[N:18][OH:19])[CH3:15])=[CH:10][C:3]=1[CH2:4][NH:5][C:6](=[O:9])[O:7][CH3:8]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 962Water2 回HCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium AcetateHCID 12151316methyl N-[(5-acetyl-2-chlorophenyl)methyl]carbamate

生成物 1

HCID 86641517methyl N-[2-chloro-5-(1-hydroxyiminoethyl)benzyl]carbamate収率 97.9%

試薬・触媒・溶媒 2

HCID 702
Ethanol
溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

5.0 g of methyl N-(2-chloro-5-acetylbenzyl)carbamate was dissolved in 10 ml of ethanol, and 1.5 g of hydroxylamine hydrochloride, 3.0 g of sodium acetate and 5 ml of water were added thereto, followed by reflux under heating for 4 hours. After completion of the reaction, water was added to the reaction mixture, extraction with ethyl acetate was carried out, the organic layer was dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The obtained crystals were washed with hexane to obtain 5.2 g of methyl N-[2-chloro-5-(1-hydroxyiminoethyl)benzyl]carbamate as colorless crystals (m.p. 124-127° C.).

後処理

  1. temperatureby reflux
  2. temperatureunder heating for 4 hours
  3. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
  4. distillationthe solvent was distilled off under reduced pressure
  5. washThe obtained crystals were washed with hexane

出典と根拠

ORDレコード
ord-11bc8b001edd4d08b3e3b87d50c5fe75
出典データセット
uspto-grants-2004_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06812229B1

反応ノート

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