Water → HCID 13776037, Verbindung

HRID 845344Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 845344
[CH2:1]([CH:13]1[CH2:18][C:17](=O)[CH2:16][CH2:15][C:14]1=O)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12].[C:21](#[N:25])[CH2:22][C:23]#[N:24].O>NCCC(O)=O.C(Cl)(Cl)Cl>[C:23]([C:22]([C:21]#[N:25])=[C:14]1[CH2:15][CH2:16][C:17](=[C:22]([C:21]#[N:25])[C:23]#[N:24])[CH2:18][CH:13]1[CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12])#[N:24]

Komponenten

6

Edukt 3

HCID 962WaterHCID 8010MalononitrileHCID 137760342-Dodecylcyclohexane-1,4-dione

Produkt 1

HCID 13776037HCID 13776037, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 239Beta-AlanineKatalysatorHCID 6212ChloroformLösungsmittel

Versuchsvorschrift

A mixture of 2 g (0.0071M) of thus obtained 2-dodecyl-1,4-cyclohexane-dione and 1.4 g (0.0212M) of malononitrile was heated in a water bath to make a solution. β-alanine as a catalyst and 2 ml of water were added to the solution and stirred at a temperature between 40° C. and 50° C. for 8 hours to react the mixture. After cooling, the reacted mixture was dissolved in chloroform, and rinsed with water and dried. The dried material was concentrated under reduced pressure, and purified through silica gel column chromatography. As a result, 1.26 g of white crystal of 1,4-bis-(dicyanomethylene)-2-dodecyl cyclohexane was obtained. The obtained compound had a melting point of 97° C. and an infrared absorption band of 2250 cm-1 which corresponds to a cyano group.

Aufarbeitung

  1. temperaturewas heated in a water bath
  2. customto react the mixture
  3. temperatureAfter cooling
  4. washrinsed with water
  5. customdried
  6. concentrationThe dried material was concentrated under reduced pressure
  7. custompurified through silica gel column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-e50fbc96f6d446cbbb52ea8bd566fba3
Quelldatensatz
uspto-grants-1988_07
Patentnummer
US04758381

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