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

HRID 545235

反応式

HRID 545235 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-bd50beb18dbb4ea389c1ea8587e0103b
出典データセット
uspto-grants-2011_05
特許番号
US07935708B2

関連ノート

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