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Quinoline → 2,7-bis(N-3-pyridylacetylamino)dibenzodioxin

HRID 905537
ノート
印刷プレビュー

反応式

HRID 905537 の反応式
[C:1]([NH:4][C:5]1[CH:22]=[CH:21][C:8]2[O:9][C:10]3[CH:16]=[C:15]([NH:17][C:18](=[O:20])[CH3:19])[CH:14]=[CH:13][C:11]=3[O:12][C:7]=2[CH:6]=1)(=[O:3])[CH3:2].I[C:24]1[CH:25]=[N:26][CH:27]=[CH:28][CH:29]=1.C(=O)([O-])[O-].[K+].[K+].[N:36]1[C:45]2[C:40](=CC=CC=2)[CH:39]=[CH:38][CH:37]=1>[Cu]I.O.C(Cl)Cl>[N:26]1[CH:27]=[CH:28][CH:29]=[C:24]([CH2:19][C:18]([NH:17][C:15]2[CH:14]=[CH:13][C:11]3[O:12][C:7]4[CH:6]=[C:5]([NH:4][C:1](=[O:3])[CH2:2][C:38]5[CH:37]=[N:36][CH:45]=[CH:40][CH:39]=5)[CH:22]=[CH:21][C:8]=4[O:9][C:10]=3[CH:16]=2)=[O:20])[CH:25]=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

8

反応物 4

HCID 7047QuinolineHCID 11430Potassium CarbonateHCID 707143-IodopyridineHCID 578925072,7-Bis(acetylamino)dibenzodioxin

生成物 1

HCID 673893532,7-bis(N-3-pyridylacetylamino)dibenzodioxin

試薬・触媒・溶媒 3

HCID 24350
Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)
触媒
HCID 962Water溶媒
HCID 6344Dichloromethane溶媒

反応条件

温度
170 °C

実験手順

A slurry prepared from 7.0 g (0.023 mole) of 2,7-bis(acetylamino)dibenzodioxin, 12.0 g (0.059 mole) of 3-iodopyridine, 9.8 g (0.051 mole) of copper (I) iodide, 12.9 g (0.093 mole) of potassium carbonate, and 230 ml of quinoline was heated with stirring at 170° C. for 48 hours. The reaction mixture was cooled to room temperature, 100 ml of methylene chloride and 100 ml of water were added, and a precipitate was separated by filtration. To the filtrate was added 100 ml of water and the organic layer was separated from the aqueous layer. The organic layer was concentrated and dried under reduced pressure to give 23.5 g of a crude product which was used without purification in the next reaction.

後処理

  1. temperaturewas heated
  2. temperatureThe reaction mixture was cooled to room temperature
  3. customa precipitate was separated by filtration
  4. additionTo the filtrate was added 100 ml of water
  5. customthe organic layer was separated from the aqueous layer
  6. concentrationThe organic layer was concentrated
  7. customdried under reduced pressure

出典と根拠

ORDレコード
ord-0ab7ca54bcbc4db89a8e7dd6e3a56049
出典データセット
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08012606B2

反応ノート

読み込み中…

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