Ethanol → 2-(3,4-Dichlorophenylthiomethyl)glutaronitrile

HRID 1885601Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1885601
[Cl:1][C:2]1[CH:3]=[C:4]([SH:9])[CH:5]=[CH:6][C:7]=1[Cl:8].[CH2:10]=[C:11]([CH2:14][CH2:15][C:16]#[N:17])[C:12]#[N:13].C(O)C>CO>[Cl:1][C:2]1[CH:3]=[C:4]([S:9][CH2:10][CH:11]([CH2:14][CH2:15][C:16]#[N:17])[C:12]#[N:13])[CH:5]=[CH:6][C:7]=1[Cl:8]

Komponenten

5

Edukt 3

HCID 702EthanolHCID 740802,4-Dicyano-1-buteneHCID 799643,4-Dichlorobenzenethiol

Produkt 1

HCID 198793522-(3,4-Dichlorophenylthiomethyl)glutaronitrile

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

A mixture of 3,4-dichlorobenzenethiol (3.00 ml), methyleneglutaronitrile (2.57 ml), ethanol (25 ml), and triton B (40% methanol solution, 10 drops) was refluxed for 4 hours. After the reaction mixture was concentrated in vacuo, the resulting residue was dissolved in chloroform, washed with water, and dried over MgSO4. The solvent was evaporated at reduced pressure, and the residue was recrystallized from diethyl ether-hexane to give 6.14 g of 2-(3,4-dichlorophenylthiomethyl)glutaronitrile.

Aufarbeitung

  1. temperaturewas refluxed for 4 hours
  2. concentrationAfter the reaction mixture was concentrated in vacuo
  3. dissolutionthe resulting residue was dissolved in chloroform
  4. washwashed with water
  5. dry with materialdried over MgSO4
  6. customThe solvent was evaporated at reduced pressure
  7. customthe residue was recrystallized from diethyl ether-hexane

Quellen und Nachweise

ORD-Eintrag
ord-6cc0bbfeb3ad4443b7da709c89e08b7d
Quelldatensatz
uspto-grants-1992_09
Patentnummer
US05145869

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