Phenyltrimethylammonium bromide dibromide → 2-Bromo-1-(5-bromo-3-(trifluoromethyl)pyridin-2-yl)ethanone

HRID 545090ノート

反応式

HRID 545090 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([C:11]([F:14])([F:13])[F:12])[C:5]([C:8](=[O:10])[CH3:9])=[N:6][CH:7]=1.[Br-:15].[Br-].[Br-].C1([N+](C)(C)C)C=CC=CC=1.C1([N+](C)(C)C)C=CC=CC=1.C1([N+](C)(C)C)C=CC=CC=1>C1COCC1>[Br:15][CH2:9][C:8]([C:5]1[C:4]([C:11]([F:14])([F:12])[F:13])=[CH:3][C:2]([Br:1])=[CH:7][N:6]=1)=[O:10]

参加物

4

反応物 2

HCID 17977687Phenyltrimethylammonium bromide dibromideHCID 586455621-(5-Bromo-3-(trifluoromethyl)pyridin-2-yl)ethanone

生成物 1

HCID 866051072-Bromo-1-(5-bromo-3-(trifluoromethyl)pyridin-2-yl)ethanone

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Dissolve 1-(5-bromo-3-(trifluoromethyl)pyridin-2-yl)ethanone (0.7 g, 0.0026 mol) in anhydrous THF at room temperature under N2 atmosphere. Add phenyltrimethyl-ammonium tribromide (1.47 g, 0.0039 moles, 1.5 eq.) to the reaction mixture and reflux overnight. Cool the reaction mixture to room temperature, filter the insoluble solid and concentrate the filtrate under vacuum. Purify by column chromatography to afford the title compound as a yellow oil.

後処理

  1. filtrationfilter the insoluble solid
  2. concentrationconcentrate the filtrate under vacuum
  3. customPurify by column chromatography

出典と根拠

ORDレコード
ord-663cd03b059e4557847927ba69c5b95b
出典データセット
uspto-grants-2011_05
特許番号
US07935702B2

反応ノート

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