Phenylacetonitrile → 2-Phenylethanethioamide

HRID 1067416Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1067416
[C:1]1([CH2:7][C:8]#[N:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.P([O-])(OCC)(SCC)=[S:11]>Cl.C(OCC)(=O)C>[C:1]1([CH2:7][C:8]([NH2:9])=[S:11])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

Komponenten

4

Edukt 2

HCID 8794PhenylacetonitrileHCID 53249491Diethyldithiophosphate

Produkt 1

HCID 7313682-PhenylethanethioamideAusbeute 55 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 21866389Hydrogen chloride-ethyl acetateLösungsmittel

Versuchsvorschrift

A solution of phenylacetonitrile (10.0 g, 85.4 mmol) and diethyl dithiophosphate (17.5 g, 93.9 mmol) in 4N-HCl/ethyl acetate (400 mL) was stirred at room temperature for 16 hours. This reaction mixture was washed with water and saturated aqueous sodium hydrogen carbonate solution, dried over MgSO4, filtered, and concentrated under reduced pressure. The residue was crystallized from ethanol to provide 7.1 g of the title compound. Yield 55%.

Aufarbeitung

  1. washThis reaction mixture was washed with water and saturated aqueous sodium hydrogen carbonate solution
  2. dry with materialdried over MgSO4
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was crystallized from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-b95e9b3ac9114e76baa3b07b56de8fcd
Quelldatensatz
uspto-grants-2001_06
Patentnummer
US06248766B1

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