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Trimethylazanium;chloride → 1-(6-Bromo-3-hydroxypyridin-2-YL)ethanone

HRID 2091249
ノート
印刷プレビュー

反応式

HRID 2091249 の反応式
[Cl-].[Al+3].[Cl-].[Cl-].[Cl-].C[NH+](C)C.C([O:17][C:18]1[C:19]([C:25](=[O:27])[CH3:26])=[N:20][C:21]([Br:24])=[CH:22][CH:23]=1)C1C=CC=CC=1>C1(C)C=CC=CC=1>[Br:24][C:21]1[N:20]=[C:19]([C:25](=[O:27])[CH3:26])[C:18]([OH:17])=[CH:23][CH:22]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 11649Trimethylazanium;chlorideHCID 6451240Aluminum(III) ChlorideHCID 866627361-(3-(Benzyloxy)-6-bromopyridin-2-yl)ethanone

生成物 1

HCID 722180151-(6-Bromo-3-hydroxypyridin-2-YL)ethanone収率 83%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

実験手順

To a suspension (30 mL) of aluminum chloride (3.96 g) in toluene was added trimethylammonium chloride (1.32 g), and the mixture was stirred under argon atmosphere at room temperature for 1 hr. A solution (30 mL) of 1-[3-(benzyloxy)-6-bromopyridin-2-yl]ethanone (2.81 g) synthesized above in toluene was added to the mixture, and the mixture was stirred at room temperature for 3 hr. The reaction mixture was concentrated under reduced pressure, saturated aqueous Rochelle salt solution was added to the residue, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, dried over magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (0-5% ethyl acetate/hexane) to give the title object compound (1.64 g, 83%) as a yellow solid.

後処理

  1. additionwas added to the mixture
  2. stirringthe mixture was stirred at room temperature for 3 hr
  3. concentrationThe reaction mixture was concentrated under reduced pressure, saturated aqueous Rochelle salt solution
  4. additionwas added to the residue
  5. extractionthe mixture was extracted with ethyl acetate
  6. washThe extract was washed with saturated brine
  7. dry with materialdried over magnesium sulfate
  8. concentrationconcentrated under reduced pressure
  9. customThe residue was purified by silica gel column chromatography (0-5% ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-a2661d90993c45eda2e624fbe304906a
出典データセット
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08436043B2

反応ノート

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