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Water → 2-Bromo-N-methyl-N-phenylacetamide

HRID 2192364
ノート
印刷プレビュー

反応式

HRID 2192364 の反応式
[CH3:1][NH:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.C(=O)([O-])[O-].[K+].[K+].[Br:15][CH2:16][C:17](Br)=[O:18].O>ClCCl>[Br:15][CH2:16][C:17]([N:2]([CH3:1])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1)=[O:18]
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 4

HCID 962WaterHCID 7515N-MethylanilineHCID 11430Potassium CarbonateHCID 61147Bromoacetyl bromide

生成物 1

HCID 344952-Bromo-N-methyl-N-phenylacetamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a mixture of N-methyl aniline (5 mL) and potassium carbonate (9.6 g) in 100 mL dichloromethane was added bromoacetyl bromide (8.1 mL) (exotherm). The mixture was stirred for 4.5h then water was added. The phases were separated and the organic layer was concentrated. The crude product was purified by silica gel chromatography eluting with 0-100% EtOAc/cyclohexane. The relevant fractions were combined and evaporated and the residue was taken up in dichloromethane and washed with water. The organic layer was stirred with another portion of water for a few minutes and then the layers were separated. Evaporation of the organic layer gave the sub-titled compound (10.2 g) as a straw coloured solid.

後処理

  1. customThe phases were separated
  2. concentrationthe organic layer was concentrated
  3. customThe crude product was purified by silica gel chromatography
  4. washeluting with 0-100% EtOAc/cyclohexane
  5. customevaporated
  6. washwashed with water
  7. customthe layers were separated
  8. customEvaporation of the organic layer

出典と根拠

ORDレコード
ord-5872088bc0a441e9ad9dacb7f454debf
出典データセット
uspto-grants-2012_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08329729B2

反応ノート

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