Hydrochloric Acid → 2-(2-hydroxymethylphenyl)-2-methoxyimino-N-methylacetamide

HRID 342183노트

반응식

HRID 342183 반응식
CO.[OH:3][CH2:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[C:11](=[N:16][O:17][CH3:18])[C:12]([NH:14][CH3:15])=[O:13].Cl.CON=C(C1C=CC=CC=1COC1CCCCO1)C(NC)=O>[Cl-].[Na+].O>[OH:3][CH2:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[C:11](=[N:16][O:17][CH3:18])[C:12]([NH:14][CH3:15])=[O:13]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 53869643HCID 53869643, 화합물HCID 867535212-(2-hydroxymethylphenyl)-2-methoxyimino-N-methylacetamide Methanol

생성물 1

HCID 544725602-(2-hydroxymethylphenyl)-2-methoxyimino-N-methylacetamide수율 94.6%

시약·촉매·용매 1

HCID 57417360Sodium chloride; water용매

실험 절차

Preparation of 2-(2-hydroxymethylphenyl)-2-methoxyimino-N-methylacetamide Methanol (2 ml) and a 36% aqueous hydrochloric acid solution (0.01 g, 0.0001 mol) were added to an E/Z mixture of 2-methoxyimino-N-methyl-2-[2-(2-tetrahydropyranyloxymethyl)phenyl]acetamide (0.31 g, 0.001 mol), and the mixture was stirred at room temperature for 30 minutes. After completion of the reaction, half-saturated brine (80 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-hydroxymethylphenyl)-2-methoxyimino-N-methylacetamide (0.21 g, Yield: 94.6%, E/Z=97/3) as colorless crystals.

후처리

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

출처 및 근거

ORD 기록
ord-d815929c9aa1476199258f8bb96ef56a
출처 데이터셋
uspto-grants-1999_01
특허 번호
US05856573

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