Reaktion #953680

ord-bd9ef1d5f664452fbb3029a3ec0b4a5d

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.DISTILLATIONThe dioxane is then distilled off
  2. 2
    SonstigeAn oil separates which crystallizes after a short while
  3. 3
    Sonstigeto give 3.2 g
  4. 4
    Sonstigeof (2-oxo-1-imidazolidinyl)carbamothioic acid, S-phenyl ester, m.p. 154°-159° (after recrystallization from ethyl acetate)

Vorschrift

3.2 ml. of (phenylthio)carbonyl chloride are dissolved in 30 ml. of dioxane and a solution of 2.63 g. of 1-amino-2-imidazolidinone in a mixture of 10 ml. of dioxane and 10 ml. of water is added. 2N sodium hydroxide solution is added dropwise at room temperature so that the pH is about 7.5-8.0. About 15 ml. of 2N sodium hydroxide are required. The dioxane is then distilled off. An oil separates which crystallizes after a short while to give 3.2 g. of (2-oxo-1-imidazolidinyl)carbamothioic acid, S-phenyl ester, m.p. 154°-159° (after recrystallization from ethyl acetate).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04099001uspto-grants-1978_07