Reaktion #50015

ord-78b65f57d4cc4543959bfb9496b3572a

Reaktionsgleichung

CC(=O)[C@@H]1CC(=S)N(C(C)=O)C1
(+)-(4R)-1-Acetyl-4-acetylthio-2-pyrrolidone
CCN(CC)CC
triethylamine
O=C(O)Cc1cccs1
thiolacetic acid
CC(=O)C1CC(=S)N(C(C)=O)C1
(±)-1-acetyl-4-acetylthio-2-pyrrolidone
Ausbeute 90.0%

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturthe mixture is refluxed for three hours
  2. 2
    WaschenThe reaction solution is washed with water
  3. 3
    Sonstigedried
  4. 4
    Sonstigeevaporated
  5. 5
    Sonstigeto remove the solvent

Vorschrift

(+)-(4R)-1-Acetyl-4-acetylthio-2-pyrrolidone (3 g) and triethylamine (2.1 ml) are dissolved in ethyl acetate (30 ml), and the mixture is refluxed for three hours, and then allowed to stand at room temperature for 8 hours. To the reaction solution is added thiolacetic acid (1.2 ml), and the mixture is stirred at room temperature for 5 hours. The reaction solution is washed with water, dried, and evaporated to remove the solvent to give (±)-1-acetyl-4-acetylthio-2-pyrrolidone (2.7 g).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05424446uspto-grants-1995_06