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Diethyl Ether → Penconazole

HRID 637516
ノート
印刷プレビュー

反応式

HRID 637516 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[CH:9]([CH2:16][CH2:17][CH3:18])[CH2:10][NH:11][NH:12][C:13](=O)C.C(OCC)C.[OH-].[Na+].[Cl-].[CH3:27][N:28](C)C=NC=[N+](C)C>C(O)C.Cl>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[CH:9]([CH2:16][CH2:17][CH3:18])[CH2:10][N:11]1[CH:27]=[N:28][CH:13]=[N:12]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

7

反応物 4

HCID 3283Diethyl EtherHCID 14798Sodium HydroxideHCID 11008255Gold's ReagentHCID 20257012HCID 20257012、化合物

生成物 1

HCID 91693Penconazole収率 86.9%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒
HCID 702
Ethanol
溶媒
2 回

反応条件

温度
170 °C

実験手順

5.1 g (0.017 mol) of 1-[2-(2,4-dichlorophenyl)pentyl]-2acetylhydrazine in 10 ml of ethanol and 10 ml of concentrated hydrochloric acid are stirred at 50° C. overnight. The reaction mixture is then distributed between diethyl ether and 2 N sodium hydroxide solution; and the residue after concentration by evaporation is refluxed in 50 ml of absolute ethanol with 5.75 g (0.035 mol) of [3-(dimethylamino)-2-aza-prop-2-en-1-ylidene]-dimethylammonium chloride for 3.5 hours. The reaction solution is then concentrated by evaporation; 50 ml of formamide are added, and the mixture is heated at 170° C. for 1.5 hours. The reaction mixture, to which water has been added, is extracted with diethyl ether, and the residue obtained after concentration by evaporation is chromatographed to yield 4.2 g (84% of theory) of 1-[2-(2,4-dichlorophenyl)-pentyl]-1H-1,2,4-triazole.

後処理

  1. concentrationand the residue after concentration
  2. customby evaporation
  3. concentrationThe reaction solution is then concentrated by evaporation
  4. addition50 ml of formamide are added
  5. additionThe reaction mixture, to which water has been added
  6. extractionis extracted with diethyl ether
  7. customthe residue obtained
  8. concentrationafter concentration
  9. customby evaporation
  10. customis chromatographed

出典と根拠

ORDレコード
ord-dd1c2a732b684b0f9df747792417a6ca
出典データセット
uspto-grants-1985_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04556717

反応ノート

読み込み中…

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