Reaktion #66056

ord-6fd1d7b397a74853bd84524d807b4c37

Reaktionsgleichung

Cl
HCl
CCCNC1CCc2nc(N)sc2C1
2-amino-4,5,6,7-tetrahydro-6-(propylamino)benzothiazole
Cl
HCl
CCCNC1CCc2nc(N)sc2C1
2-amino-4,5,6,7-tetrahydro-6-(propylamino)benzothiazole
CCCNC1CCc2nc(N)sc2C1.Cl.Cl
2-amino-4,5,6,7-tetrahydro-6-(propylamino)benzothiazole dihydrochloride salt

Lösungsmittel

Reaktionsbedingungen

Temperatur
15°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeHCl (gas) may be bubbled into the slurry for about 1 hour
  2. 2
    Filtrationafter which the mixture may be filtered
  3. 3
    Waschenwashed with IPAC
  4. 4
    Sonstigedried under vacuum at room temperature

Vorschrift

An alternate method for conversion of the sulfonate or halide salts of 2-amino-4,5,6,7-tetrahydro-6-(propylamino)benzothiazole to an HCl salt involves the use of a concentrated solution of HCl and isopropyl acetate (IPAC). A sulfonate or halide salt of 2-amino-4,5,6,7-tetrahydro-6-(propylamino)benzothiazole may be taken up in IPAC and cooled to 15° C. HCl (gas) may be bubbled into the slurry for about 1 hour, after which the mixture may be filtered, washed with IPAC and dried under vacuum at room temperature to afford a 2-amino-4,5,6,7-tetrahydro-6-(propylamino)benzothiazole dihydrochloride salt. A detailed example of this synthesis may be found in Example 9.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08524695B2uspto-grants-2013_09