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Ethyl Acetate → N-acetoxyacetyl-N-(2-methoxybenzyl)-2-phenoxyaniline

HRID 1016577
ノート
印刷プレビュー

反応式

HRID 1016577 の反応式
Cl[CH2:2][C:3]([N:5]([CH2:19][C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=1[O:26][CH3:27])[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[O:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)=[O:4].[C:28]([O-:31])(=[O:30])[CH3:29].[Na+].C(OCC)(=O)C>C1C=CC=CC=1.[Br-].C([N+](CCCC)(CCCC)CCCC)CCC>[C:28]([O:31][CH2:2][C:3]([N:5]([CH2:19][C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=1[O:26][CH3:27])[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[O:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)=[O:4])(=[O:30])[CH3:29]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 8857Ethyl AcetateHCID 517045Sodium AcetateHCID 18407214HCID 18407214、化合物

生成物 1

HCID 18407208N-acetoxyacetyl-N-(2-methoxybenzyl)-2-phenoxyaniline収率 96%

試薬・触媒・溶媒 2

HCID 74236Tetrabutylammonium Bromide触媒HCID 241Benzene
溶媒

実験手順

In 10 ml of benzene were stirred 1.01 g of N-chloroacetyl-N-(2-methoxybenzyl)-2-phenoxyaniline, 1.30 g of sodium acetate and 170 mg of tetra-n-butyl ammonium bromide at 80° C. for 5 hours. The reaction mixture was poured into ethyl acetate, washed with water and a saturated aqueous sodium chloride solution, successively, and dried over anhydrous sodium sulfate. After removal of the drying agent by filtration, the solvent was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (eluent; ethyl acetate−hexane=1:3) to give 1.03 g of N-acetoxyacetyl-N-(2-methoxybenzyl)-2-phenoxyaniline as an oil.

後処理

  1. washwashed with water
  2. dry with materiala saturated aqueous sodium chloride solution, successively, and dried over anhydrous sodium sulfate
  3. customAfter removal of the drying agent
  4. filtrationby filtration
  5. concentrationthe solvent was concentrated under reduced pressure
  6. customthe residue was purified by silica gel column chromatography (eluent; ethyl acetate−hexane=1:3)

出典と根拠

ORDレコード
ord-8c0ba9defba84a779439d9e1c6edc159
出典データセット
uspto-grants-2002_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06476056B2

反応ノート

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