Reaktion #3348

ord-9a24f90cc7884da083a28d124bc01ed8

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Einengenconcentrated in vacuo
  2. 2
    workup.ADDITIONThe residue was treated
  3. 3
    Sonstigepurified by column chromatography (CHCl3)
  4. 4
    SonstigeRecrystallization from diethyl ether-n-hexane

Vorschrift

Initially, 0.65 g of 2-dimethylaminobenzylchloride hydrochloride was added to a solution of 0.7 g of 2-benzylthio-5,5-dimethylimidazolin-4-thione in 20 mL of ethanol (EtOH). The reaction mixture was stirred at the room temperature for one hour, and concentrated in vacuo. The residue was treated following the procedure used in Example 62, and purified by column chromatography (CHCl3). Recrystallization from diethyl ether-n-hexane gave 2-benzylthio-4-(2-dimethylaminobenzylthio)-5,5-dimethyl-5H-imidazole in the form of a needle-like crystal. The yield of this compound was 0.75 g with a yield ratio of 72.2%, and the melting point was 91°-92° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05733922uspto-grants-1998_03