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Phenyltrimethylammonium bromide dibromide → 2-Bromo-1-(3,5-dichloropyridin-2-yl)ethanone

HRID 55976
ノート
印刷プレビュー

反応式

HRID 55976 の反応式
[Cl:1][C:2]1[C:3]([C:9](=[O:11])[CH3:10])=[N:4][CH:5]=[C:6]([Cl:8])[CH:7]=1.[Br-:12].[Br-].[Br-].C[N+](C)(C)C1C=CC=CC=1.C[N+](C1C=CC=CC=1)(C)C.C[N+](C1C=CC=CC=1)(C)C>O1CCCC1>[Br:12][CH2:10][C:9]([C:3]1[C:2]([Cl:1])=[CH:7][C:6]([Cl:8])=[CH:5][N:4]=1)=[O:11]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 17977687Phenyltrimethylammonium bromide dibromideHCID 217121631-(3,5-Dichloropyridin-2-yl)ethanone

生成物 1

HCID 534166072-Bromo-1-(3,5-dichloropyridin-2-yl)ethanone収率 161.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To 5.00 g of 1-(3,5-dichloropyridin-2-yl)ethanone in 75 ml of tetrahydrofuran, 9.94 g of trimethylphenylammonium tribromide was added, and the mixture was stirred at room temperature for 16 hours. After completion of the reaction, the precipitated solid was filtered off through celite, and the solvent was evaporated under reduced pressure. The resulting residue was purified by silica gel column chromatography using ethyl acetate-hexane (with a gradient of from 5:95 to 15:85) as the eluent to obtain 6.64 g of the desired product as a brown oil.

後処理

  1. customAfter completion of the reaction
  2. filtrationthe precipitated solid was filtered off through celite
  3. customthe solvent was evaporated under reduced pressure
  4. customThe resulting residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-cd850f646e874edab909d8c8af2c313c
出典データセット
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09434684B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート