Reaktion #4930

ord-899dfc4eb3d343fca6a7503b6a131990

Reaktionsgleichung

CNC
dimethylamine
CN1CC(CCCl)Sc2ncccc2C1=O
2-(2-chloroethyl)-2,3-dihydro-4-methylpyrido[3,2-f][1,4]-thiazepin-5(4H)-one
CNC
dimethylamine
CN(C)CCC1CN(C)C(=O)c2cccnc2S1.Cl.Cl
2-[2-(Dimethylamino)ethyl]-2,3-dihydro-4-methylpyrido[3,2-f][1,4]-thiazepin-5(4H)-one dihydrochloride

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeto evaporate
  2. 2
    Sonstigethe residue was partitioned between chloroform and dilute sodium hydroxide
  3. 3
    EinengenThe chloroform layer was concentrated
  4. 4
    workup.DISSOLUTIONthe residue, the free base of the title compound, was dissolved in isopropyl alcohol
  5. 5
    Sonstigereacted with hydrogen chloride

Vorschrift

A solution of 1.5 g (0.0058 mole) of 2-(2-chloroethyl)-2,3-dihydro-4-methylpyrido[3,2-f][1,4]-thiazepin-5(4H)-one in 20 ml of dimethylamine was stirred at 25° C. in a sealed container for 72 hr. The excess dimethylamine was allowed to evaporate and the residue was partitioned between chloroform and dilute sodium hydroxide. The chloroform layer was concentrated and the residue, the free base of the title compound, was dissolved in isopropyl alcohol and reacted with hydrogen chloride. The resulting hydrochloride salt weighted 1.5 g (77%), m.p.>250° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04727152uspto-grants-1988_02