Reaktion #50016

Reaktionsgleichung

phosphorus pentasulfide

(4R)-4-Acetylthio-2-pyrrolidone

water

ethyl acetate

→

(+)-(4R)-4-acetylthiopyrrolidine-2-thione

Ausbeute 72.0%

Lösungsmittel

toluene

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGthe mixture is stirred at room temperature for 1.5 hour
2. 2
   SonstigeThe insoluble materials are removed by filtration
3. 3
   Waschenthe organic layer is washed with water
4. 4
   Sonstigedried
5. 5
   Sonstigeevaporated
6. 6
   Sonstigeto remove the solvent
7. 7
   SonstigeThe residue is recrystallized from toluene

Vorschrift

(4R)-4-Acetylthio-2-pyrrolidone (10 g) is dissolved in toluene (100 ml), and thereto is added gradually phosphorus pentasulfide (9.5 g), and the mixture is stirred at room temperature for 20 minutes. To the reaction solution are added water and ethyl acetate, and the mixture is stirred at room temperature for 1.5 hour. The insoluble materials are removed by filtration, and the organic layer is washed with water, dried, and evaporated to remove the solvent. The residue is recrystallized from toluene to give (+)-(4R)-4-acetylthiopyrrolidine-2-thione (7.9 g).

Quelle