Dimethylformamide → 2-(3-Chlorophenoxymethyl)-alpha-methoxyiminobenzyl chloride

HRID 1004349노트

반응식

HRID 1004349 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([OH:8])[CH:5]=[CH:6][CH:7]=1.[CH3:9]N(C)C=O.C(=O)([O-])[O-].[K+].[K+].[CH3:20][O:21][N:22]=[C:23]([Cl:30])[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1>CCOCC>[Cl:1][C:2]1[CH:3]=[C:4]([CH:5]=[CH:6][CH:7]=1)[O:8][CH2:9][C:29]1[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=1[C:23]([Cl:30])=[N:22][O:21][CH3:20]

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 79333-ChlorophenolHCID 11430Potassium CarbonateHCID 85442083alpha-Methoxyiminobenzyl chloride

생성물 1

HCID 544326462-(3-Chlorophenoxymethyl)-alpha-methoxyiminobenzyl chloride수율 91.2%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

3-Chlorophenol (3.09 g, 0.024 mol), N,N-dimethylformamide (20 ml) and potassium carbonate (4.15 g, 0.03 mol) were added to 2-chloromethyl-(α-methoxyiminobenzyl chloride (4.36 g, 0.02 mol), and the mixture was stirred at room temperature for 4 days. After completion of the reaction, ether (250 ml) was added, and the mixture was washed with brine (200 ml) twice. The ether layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was purified by silica gel chromatography (ethyl acetate/n-hexane) to give 2-(3-chlorophenoxymethyl)-α-methoxyiminobenzyl chloride (5.66 g, 91.2%) as a colorless oil.

후처리

  1. additionwas added
  2. washthe mixture was washed with brine (200 ml) twice
  3. dry with materialThe ether layer was dried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was purified by silica gel chromatography (ethyl acetate/n-hexane)

출처 및 근거

ORD 기록
ord-a5b8089be2084b34adfe96721c613871
출처 데이터셋
uspto-grants-2000_04
특허 번호
US06048885

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