Water → 4-[Ethyl(methyl)amino]benzaldehyde

HRID 1663604노트

반응식

HRID 1663604 반응식
F[C:2]1[CH:9]=[CH:8][C:5]([CH:6]=[O:7])=[CH:4][CH:3]=1.[CH3:10][NH:11][CH2:12][CH3:13].C(=O)([O-])[O-].[K+].[K+].O>CS(C)=O>[CH2:12]([N:11]([C:2]1[CH:9]=[CH:8][C:5]([CH:6]=[O:7])=[CH:4][CH:3]=1)[CH3:10])[CH3:13]

참가 물질

6

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 12219N-MethylethylamineHCID 680234-Fluorobenzaldehyde

생성물 1

HCID 133962824-[Ethyl(methyl)amino]benzaldehyde수율 89%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

To a solution of 4-fluorobenzaldehyde (1.5 g) and methylethylamine (1.56 mL) in dimethylsulfoxide (9 mL) was added potassium carbonate (2.17 g) and the mixture was stirred by using a microwave synthesizer (Biotage LTD.) at 120° C. for 2 hours. Thereto was added water and the mixture was extracted with ethyl acetate. The extract was dried over magnesium sulfate and concentrated in vacuo. The resultant crude product was purified by a column chromatography on silica gel (solvent; hexane/ethyl acetate=95:5→80:20) to give 4-(N-ethyl-N-methylamino)benzaldehyde (1.89 g, yield: 89%).

후처리

  1. customat 120° C.
  2. customfor 2 hours
  3. extractionthe mixture was extracted with ethyl acetate
  4. dry with materialThe extract was dried over magnesium sulfate
  5. concentrationconcentrated in vacuo
  6. customThe resultant crude product was purified by a column chromatography on silica gel (solvent; hexane/ethyl acetate=95:5→80:20)

출처 및 근거

ORD 기록
ord-5ed1b6e0df1f4b21b7ae5f6f131b099c
출처 데이터셋
uspto-grants-2011_10
특허 번호
US08034949B2

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