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Selenium Dioxide → HCID 21847014、化合物

HRID 619682
ノート
印刷プレビュー

反応式

HRID 619682 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=[O:16])[CH2:9][C:10]2[CH:15]=[CH:14][N:13]=[CH:12][CH:11]=2)=[CH:4][CH:3]=1.[Se](=O)=[O:18]>O1CCOCC1>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=[O:16])[C:9]([C:10]2[CH:15]=[CH:14][N:13]=[CH:12][CH:11]=2)=[O:18])=[CH:4][CH:3]=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

4

反応物 2

HCID 24007Selenium DioxideHCID 103990241-(4-Chloro-phenyl)-2-pyridin-4-YL-ethanone

生成物 1

HCID 21847014HCID 21847014、化合物収率 89.4%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
100 °C

実験手順

A solution of 25 g of 1-(4-chlorophenyl)-2-pyridin-4-yl-ethanone in 285 ml of dioxan was treated with 20 g of selenium dioxide. The mixture was stirred at 100° C. for 1 hour and filtered. The solvent was evaporated and the residue was dissolved in dichloromethane. The solution was washed three times with water, dried over anhydrous magnesium sulphate and evaporated. The residue was dissolved in ethyl acetate, the solution was filtered over silica gel and evaporated to yield 23.7 g of 1-(4-chlorophenyl)-2-pyridin-4-yl-ethanedione, m.p. 119-120° C.

後処理

  1. filtrationfiltered
  2. customThe solvent was evaporated
  3. dissolutionthe residue was dissolved in dichloromethane
  4. washThe solution was washed three times with water
  5. dry with materialdried over anhydrous magnesium sulphate
  6. customevaporated
  7. dissolutionThe residue was dissolved in ethyl acetate
  8. filtrationthe solution was filtered over silica gel
  9. customevaporated

出典と根拠

ORDレコード
ord-9a69dc3e69de49eaa72b899978a8486c
出典データセット
uspto-grants-1999_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05959113

反応ノート

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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