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Methanol → 4-(3-Chloropyridin-2-yl)benzaldehyde

HRID 578590
ノート
印刷プレビュー

反応式

HRID 578590 の反応式
[Cl:1][C:2]1[C:3]([C:8]2[CH:13]=[CH:12][C:11]([CH3:14])=[CH:10][CH:9]=2)=[N:4][CH:5]=[CH:6][CH:7]=1.C[OH:16]>>[Cl:1][C:2]1[C:3]([C:8]2[CH:13]=[CH:12][C:11]([CH:14]=[O:16])=[CH:10][CH:9]=2)=[N:4][CH:5]=[CH:6][CH:7]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

3

反応物 2

HCID 887Methanol2 回HCID 207099363-Chloro-2-(p-tolyl)pyridine

生成物 1

HCID 534262384-(3-Chloropyridin-2-yl)benzaldehyde収率 60%

反応条件

温度
25 °C

実験手順

{circle around (2)} 100 g (0.49 mol) of 3-chloro-2-para-tolylpyridine was dissolved in 0.5 L of methanol in a reactor. A solution of 537 g (0.98 mol) of ceric ammonium nitrate in 1 L of methanol was added dropwise, and the mixture was refluxed for 4˜6 hours. The reaction solution was cooled to 25° C. and concentrated under reduced pressure. A 10% sodium bicarbonate solution was added, and the mixture was extracted with ethyl acetate. The organic layer was dried with magnesium sulfate, and concentrated under reduced pressure, yielding 4-(3-chloropyridin-2-yl)benzaldehyde as represented below in a 60% yield.

後処理

  1. temperaturethe mixture was refluxed for 4˜6 hours
  2. concentrationconcentrated under reduced pressure
  3. additionA 10% sodium bicarbonate solution was added
  4. extractionthe mixture was extracted with ethyl acetate
  5. dry with materialThe organic layer was dried with magnesium sulfate
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-c844a60fb1634e37b5a567e14fc4bad1
出典データセット
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09040572B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート