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

HRID 1857818노트

반응식

HRID 1857818 반응식
CO.Cl.[CH3:4][O:5][N:6]=[C:7]([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[CH2:18][O:19]C1CCCCO1)[C:8]([NH:10][CH3:11])=[O:9]>[Cl-].[Na+].O>[OH:19][CH2:18][C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][C:12]=1[C:7](=[N:6][O:5][CH3:4])[C:8]([NH:10][CH3:11])=[O:9]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 887MethanolHCID 53869643HCID 53869643, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 57417360Sodium chloride; water용매

실험 절차

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-c185cc7c436440ff96d1c8d3080623bf
출처 데이터셋
uspto-grants-2000_11
특허 번호
US06147231

반응 노트

불러오는 중…