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Acetonitrile → HCID 86719698、化合物

HRID 922667
ノート
印刷プレビュー

反応式

HRID 922667 の反応式
[Cl:1][C:2]1[N:3]=[CH:4][NH:5][C:6]=1[Cl:7].[OH-].[K+].Br[CH2:11][C:12]1[CH:25]=[CH:24][C:23]2[C:14](=[CH:15][C:16]3[C:21]([CH:22]=2)=[CH:20][CH:19]=[CH:18][CH:17]=3)[CH:13]=1.[C:26](#[N:28])[CH3:27]>>[Cl-:1].[CH:13]1[C:14]2[C:23](=[CH:22][C:21]3[C:16]([CH:15]=2)=[CH:17][CH:18]=[CH:19][CH:20]=3)[CH:24]=[CH:25][C:12]=1[CH2:11][N+:3]1[C:2]([Cl:1])=[C:6]([Cl:7])[N:5]([CH2:27][C:26]2[CH:16]=[CH:15][C:14]3[C:13](=[CH:12][CH:25]=[CH:24][CH:23]=3)[N:28]=2)[CH:4]=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 4

HCID 6342Acetonitrile2 回HCID 14797Potassium Hydroxide2 回HCID 1400184,5-DichloroimidazoleHCID 190129612-(Bromomethyl)anthracene

生成物 1

HCID 86719698HCID 86719698、化合物

実験手順

4,5-Dichloroimidazole (0.18 g, 1.33 mmol) and potassium hydroxide (0.08 g, 1.46 mmol) will be dissolved in a minimum volume of acetonitrile and stirred at reflux for 30 min. 2-(Bromomethyl)anthracene (2.71 g, 10.0 mmol) will be added and the mixture will be returned to reflux for 3 h. The mixture will be filtered hot to remove the KBr generated. A solution of 2-(chloromethyl)quinoline will be prepared by combining 2-(chloromethyl)quinolone hydrochloride (2.14 g, 10 mmol) and potassium hydroxide (0.56 g, 10.0 mmol) in acetonitrile and refluxing the mixture for 30 min, and this solution will be added to the filtrate. The combined mixture will be returned to reflux for 6 h. The volatile components will be removed under reduced pressure, and the resulting solid will be washed with water to remove the KCl generated in the neutralization of the quinoline. The remaining solid will be dried and will be the product.

後処理

  1. temperatureat reflux for 30 min
  2. temperatureto reflux for 3 h
  3. filtrationThe mixture will be filtered hot
  4. customto remove the KBr
  5. customA solution of 2-(chloromethyl)quinoline will be prepared
  6. temperaturerefluxing the mixture for 30 min
  7. additionthis solution will be added to the filtrate
  8. temperatureto reflux for 6 h
  9. customThe volatile components will be removed under reduced pressure
  10. washthe resulting solid will be washed with water
  11. customto remove the KCl
  12. customThe remaining solid will be dried

出典と根拠

ORDレコード
ord-24e7e9f1597b4a7e8a341ebac347d5b2
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09278951B2

反応ノート

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