Bromoacetyl bromide → 2-Bromo-N-(5-chloro-2,4-dimethoxy-phenyl)-acetamide

HRID 472744ノート

反応式

HRID 472744 の反応式
[Cl:1][C:2]1[C:3]([O:11][CH3:12])=[CH:4][C:5]([O:9][CH3:10])=[C:6]([CH:8]=1)[NH2:7].[Br:13][CH2:14][C:15](Br)=[O:16]>C(Cl)Cl.O>[Br:13][CH2:14][C:15]([NH:7][C:6]1[CH:8]=[C:2]([Cl:1])[C:3]([O:11][CH3:12])=[CH:4][C:5]=1[O:9][CH3:10])=[O:16]

参加物

5

反応物 2

HCID 61147Bromoacetyl bromideHCID 668075-Chloro-2,4-dimethoxyaniline

生成物 1

HCID 636790772-Bromo-N-(5-chloro-2,4-dimethoxy-phenyl)-acetamide

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

A cooled (0° C.) solution of 5-chloro-2,4-dimethoxyaniline (5 g) in DCM under an atmosphere of argon is treated dropwise with bromoacetyl bromide (2.4 ml). After 5 minutes, TEA (7.5 ml) is added dropwise and after stirring for 20 minutes the reaction mixture is diluted with water and extracted with DCM). The organic phase is washed with distilled water, dried over Na2SO4, filtered and evaporated to give a beige solid. This is purified by flash column chromatography on silica, eluting with 20-100% n-hexane in DCM to afford the title compound. [M+H]+ 308.

後処理

  1. extractionextracted with DCM)
  2. washThe organic phase is washed with distilled water
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. customevaporated
  6. customto give a beige solid
  7. customThis is purified by flash column chromatography on silica
  8. washeluting with 20-100% n-hexane in DCM

出典と根拠

ORDレコード
ord-d24860c1302645419740632b7d2771f1
出典データセット
uspto-grants-2014_01
特許番号
US08633211B2

反応ノート

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