Reaktion #572858

ord-72ea882ea2514dae82e9df00c53157ea

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeA solution was prepared from 0.15 g
  2. 2
    Filtrationthe ethereal suspension filtered
  3. 3
    SonstigeThe solid was then recrystallized from a methanol/ether solvent mixture
  4. 4
    Sonstigeto give
  5. 5
    Sonstigepurified trans-(±)-2-acetylamino-5-n-propyl-4,4a,5,6,7,8,8a,9-octahydrothiazolo[4,5-g]quinoline hydrochloride

Vorschrift

A solution was prepared from 0.15 g. of trans-(±)-2-amino-5-n-propyl-4,4a,5,6,7,8,8a,9-octahydrothiazolo[4,5-g]quinoline (from Example 1) in 3 ml. of tetrahydrofuran (THF) to which has been added two drops of dimethylformamide (DMF). Five hundredths milliliters of acetyl chloride were added and the solution stirred at room temperature for 15 minutes. In time, the reaction mixture became a solid colorless mass. The solid was suspended in ether and the ethereal suspension filtered. The solid was then recrystallized from a methanol/ether solvent mixture to give purified trans-(±)-2-acetylamino-5-n-propyl-4,4a,5,6,7,8,8a,9-octahydrothiazolo[4,5-g]quinoline hydrochloride; yield=30.3%; melting point above 200° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04537893uspto-grants-1985_08