Ethanol → 3-Amino-5-ethyl-1-phenyl-2-pyrazoline

HRID 1388734Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1388734
[Na].[C:2]1([NH:8][NH2:9])[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C/[C:11](=[CH:14]\[CH3:15])/[C:12]#[N:13].[CH2:16](O)C>>[NH2:13][C:12]1[CH2:11][CH:14]([CH2:15][CH3:16])[N:8]([C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)[N:9]=1

Komponenten

5

Edukt 4

HCID 702EthanolHCID 7516PhenylhydrazineHCID 5355732(E)-2-Methyl-2-butenenitrileHCID 5360545Sodium

Produkt 1

HCID 130641963-Amino-5-ethyl-1-phenyl-2-pyrazoline

Versuchsvorschrift

A 0.23 g. amount of sodium metal is dissolved in 75.0 ml. of absolute ethanol, then 10.8 g. of phenylhydrazine is added, followed in 5 minutes by 3.6 g. of α-methylcrotononitrile. The reaction mixture is refluxed for 18 hours, then is evaporated to dryness in vacuo. Water is added to give a gum which solidifies on standing for 16 hours. The solid is collected and dissolved in dichloromethane. The procedure of Example 15 is continued to give 1.6 g. of the desired product as light yellow crystals, m.p. 123°-125° C.

Aufarbeitung

  1. temperatureThe reaction mixture is refluxed for 18 hours
  2. customis evaporated to dryness in vacuo
  3. additionWater is added
  4. customto give a gum which
  5. waiton standing for 16 hours
  6. customThe solid is collected
  7. dissolutiondissolved in dichloromethane
  8. customto give 1.6 g

Quellen und Nachweise

ORD-Eintrag
ord-5b4f1379201d4904beff940485c56d67
Quelldatensatz
uspto-grants-1984_02
Patentnummer
US04432991

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