2-Methyl-4-nitrophenol → Dimethyl{2-[(2-methyl-4-nitrophenyl)oxy]ethyl}amine

HRID 545235

반응식

HRID 545235 반응식
[CH3:1][C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[CH:5]=[CH:4][C:3]=1[OH:11].[CH3:12][N:13]([CH3:17])[CH2:14][CH2:15]Cl.C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[CH3:12][N:13]([CH2:14][CH2:15][O:11][C:3]1[CH:4]=[CH:5][C:6]([N+:8]([O-:10])=[O:9])=[CH:7][C:2]=1[CH3:1])[CH3:17]

참가 물질

5

반응물 3

HCID 74422-Methyl-4-nitrophenolHCID 79012-Chloro-N,N-dimethylethylamineHCID 11430Potassium Carbonate

생성물 1

HCID 58377223Dimethyl{2-[(2-methyl-4-nitrophenyl)oxy]ethyl}amine수율 20.5%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

Acetonitrile (30 mL) solution of 2 g of 2-methyl-4-nitrophenol, 1.87 g of 2-dimethylaminoethyl chloride and 5.4 g of potassium carbonate was stirred at 120° C. for 23 hours. The reaction liquid was concentrated under reduced pressure, and the residue was dissolved in ethyl acetate. The organic layer was washed with water, and dried with anhydrous sodium sulfate. The solvent was evaporated away under reduced pressure, and the crude product was purified through silica gel column chromatography (chloroform/methanol) to obtain 600 mg of the entitled compound as a white solid.

후처리

  1. customThe reaction liquid
  2. concentrationwas concentrated under reduced pressure
  3. dissolutionthe residue was dissolved in ethyl acetate
  4. washThe organic layer was washed with water
  5. dry with materialdried with anhydrous sodium sulfate
  6. customThe solvent was evaporated away under reduced pressure
  7. customthe crude product was purified through silica gel column chromatography (chloroform/methanol)

출처 및 근거

ORD 기록
ord-bd50beb18dbb4ea389c1ea8587e0103b
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07935708B2

연결된 노트

불러오는 중…