Benzaldehyde → HCID 20296018, Verbindung

HRID 1389930

Reaktionsgleichung

Reaktionsgleichung von HRID 1389930
[CH:1](=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Cl:9][C:10]1[CH:15]=[C:14]([Cl:16])[C:13]([Cl:17])=[CH:12][C:11]=1[NH2:18].[C-:19]#[N:20].[K+]>[Cl-].[Zn+2].[Cl-].O>[Cl:9][C:10]1[CH:15]=[C:14]([Cl:16])[C:13]([Cl:17])=[CH:12][C:11]=1[NH:18][CH:1]([C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)[C:19]#[N:20]

Komponenten

6

Edukt 3

HCID 240BenzaldehydeHCID 9032Potassium CyanideHCID 124872,4,5-Trichloroaniline

Produkt 1

HCID 20296018HCID 20296018, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 3007855ZincchlorideKatalysatorHCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

To a stirred mixture of 53 parts of benzaldehyde in 820 parts of water are added successively 78.6 parts of 2,4,5-trichlorobenzenamine, 81.8 parts of zinc chloride and 32.6 parts of potassium cyanide and the whole is stirred for 18 hours at 50° C. The reaction mixture is cooled to room temperature. The precipitated product is filtered off, triturated in 1000 parts of water, filtered off again and dissolved in 750 parts of trichloromethane. The solution is washed twice with water, dried, filtered and evaporated. The solid residue is triturated in petroleum ether, filtered off again and dried, yielding 83.1 parts of α-[(2,4,5-trichlorophenyl)amino]benzeneacetonitrile; mp. 123.7° C.

Aufarbeitung

  1. temperatureThe reaction mixture is cooled to room temperature
  2. filtrationThe precipitated product is filtered off
  3. customtriturated in 1000 parts of water
  4. filtrationfiltered off again
  5. dissolutiondissolved in 750 parts of trichloromethane
  6. washThe solution is washed twice with water
  7. customdried
  8. filtrationfiltered
  9. customevaporated
  10. customThe solid residue is triturated in petroleum ether
  11. filtrationfiltered off again
  12. customdried

Quellen und Nachweise

ORD-Eintrag
ord-d1698bafec5a4e2fb43185c9e8bd4d09
Quelldatensatz
uspto-grants-1981_01
Patentnummer
US04246429

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