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

HRID 2414254
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HRID 2414254 반응식
[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]
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참가 물질

7

반응물 4

HCID 962Water2회HCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium AcetateHCID 12151316methyl N-[(5-acetyl-2-chlorophenyl)methyl]carbamate

생성물 1

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

시약·촉매·용매 2

HCID 702
Ethanol
용매
HCID 8857Ethyl Acetate용매

실험 절차

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.).

후처리

  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

출처 및 근거

ORD 기록
ord-11bc8b001edd4d08b3e3b87d50c5fe75
출처 데이터셋
uspto-grants-2004_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06812229B1

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