4-Nitrophenol → Methyl (4-nitrophenoxy)acetate

HRID 482515ノート

反応式

HRID 482515 の反応式
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([OH:10])=[CH:6][CH:5]=1)([O-:3])=[O:2].Br[CH2:12][C:13]([O:15][CH3:16])=[O:14].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([O:10][CH2:12][C:13]([O:15][CH3:16])=[O:14])=[CH:6][CH:5]=1)([O-:3])=[O:2]

参加物

5

反応物 3

HCID 9804-NitrophenolHCID 11430Potassium CarbonateHCID 60984Methyl bromoacetate

生成物 1

HCID 700522Methyl (4-nitrophenoxy)acetate収率 74.5%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 56 g of 4-nitrophenol, 90 g of methyl bromoacetate, 100 g of potassium carbonate and 500 ml of dimethylformamide was stirred at room temperature for 2 days. At the end of this time, the solvent was removed by distillation under reduced pressure. The resulting residue was mixed with water and the aqueous mixture was extracted with ethyl acetate. The extract was washed with water and dried over anhydrous sodium sulfate, after which the solvent was removed by distillation under reduced pressure. The resulting residue was triturated with hexane to give 63.3 g of the title compound, melting at 98-99° C.

後処理

  1. customAt the end of this time, the solvent was removed by distillation under reduced pressure
  2. additionThe resulting residue was mixed with water
  3. extractionthe aqueous mixture was extracted with ethyl acetate
  4. washThe extract was washed with water
  5. dry with materialdried over anhydrous sodium sulfate
  6. customafter which the solvent was removed by distillation under reduced pressure
  7. customThe resulting residue was triturated with hexane

出典と根拠

ORDレコード
ord-9aafb63e5ac64ee4bfd4335bbfc2c594
出典データセット
uspto-grants-1998_08
特許番号
US05798375

反応ノート

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