Potassium thiocyanate → HCID 10655699, Verbindung

HRID 274286Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 274286
Cl[CH2:2][CH2:3][C:4]([CH3:11])([CH3:10])[C:5]([O:7][CH2:8][CH3:9])=[O:6].[S-:12][C:13]#[N:14].[K+]>CN(C)C=O.O>[CH3:10][C:4]([CH3:11])([CH2:3][CH2:2][S:12][C:13]#[N:14])[C:5]([O:7][CH2:8][CH3:9])=[O:6]

Komponenten

5

Edukt 2

HCID 516872Potassium thiocyanateHCID 10797430Ethyl 4-chloro-2,2-dimethylbutanoate

Produkt 1

HCID 10655699HCID 10655699, VerbindungAusbeute 65,9 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

In 100 ml of dimethylformamide were dissolved 22.1 g of ethyl 4-chloro-2,2-dimethylbutyrate and 14.5 g of potassium thiocyanate and the solution was stirred at 100° C. for 7 hours. The reaction mixture was poured in 500 ml of water and extracted with ethyl ether. The extract was washed with water and dried (MgSO4) and the solvent was distilled off. The residue was subjected to vacuum distillation to provide 16.4 g of the title compound as colorless oil. b.p. 109°-111° C./0.3 mmHg

Aufarbeitung

  1. extractionextracted with ethyl ether
  2. washThe extract was washed with water
  3. dry with materialdried (MgSO4)
  4. distillationthe solvent was distilled off
  5. distillationThe residue was subjected to vacuum distillation

Quellen und Nachweise

ORD-Eintrag
ord-523cc06023b34faaad3d5774d551a396
Quelldatensatz
uspto-grants-1995_02
Patentnummer
US05389633

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