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Diethyl Ether → Penconazole

HRID 637516
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HRID 637516 반응식
[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
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 3283Diethyl EtherHCID 14798Sodium HydroxideHCID 11008255Gold's ReagentHCID 20257012HCID 20257012, 화합물

생성물 1

HCID 91693Penconazole수율 86.9%

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매
HCID 702
Ethanol
용매
2회

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온도
170 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-dd1c2a732b684b0f9df747792417a6ca
출처 데이터셋
uspto-grants-1985_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04556717

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