Hydroxylamine → 2-[2-{(1-ethoxyethyl)oxymethyl}phenyl]-2-hydroxyimino-N-methylacetamide

HRID 1857815노트

반응식

HRID 1857815 반응식
CO.[NH2:3][OH:4].[CH2:5]([O:7][CH:8]([O:10][CH2:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[C:18](=O)[C:19]([NH:21][CH3:22])=[O:20])[CH3:9])[CH3:6]>O>[CH2:5]([O:7][CH:8]([O:10][CH2:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[C:18](=[N:3][OH:4])[C:19]([NH:21][CH3:22])=[O:20])[CH3:9])[CH3:6]

참가 물질

5

반응물 3

HCID 787HydroxylamineHCID 887MethanolHCID 154837862-[2-{(1-ethoxyethyl)oxymethyl}phenyl)-N-methyl-2-oxoacetamide

생성물 1

HCID 738666042-[2-{(1-ethoxyethyl)oxymethyl}phenyl]-2-hydroxyimino-N-methylacetamide수율 37.5%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Methanol (4 ml) and 50% aqueous hydroxylamine solution (0.4 g, 0.006 mol) were added to 2-[2-{(1-ethoxyethyl)oxymethyl}phenyl]-N-methyl-2-oxoacetamide (0.53 g, 0.002 mol). The mixture was stirred under reflux for 5 hours. After completion of the reaction, water (100 ml) was added, and the mixture was extracted with dichloromethane (50 ml) twice. The extract was dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The resulting residue was purified by silica gel chromatography (ethyl acetate/n-hexane) to obtain 2-[2-{(1-ethoxyethyl)oxymethyl}phenyl]-2-hydroxyimino-N-methylacetamide (Isomer A: 0.21 g (Yield: 37.5%), colorless oil; Isomer B: 0.14 g (Yield: 25.0%), colorless crystals).

후처리

  1. temperatureunder reflux for 5 hours
  2. additionwas added
  3. extractionthe mixture was extracted with dichloromethane (50 ml) twice
  4. dry with materialThe extract was dried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe resulting residue was purified by silica gel chromatography (ethyl acetate/n-hexane)

출처 및 근거

ORD 기록
ord-ea2648f3a65e43a18e2f62bff33909a0
출처 데이터셋
uspto-grants-2000_11
특허 번호
US06147231

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