Reaktion #505530

Reaktionsgleichung

(S)-4,5,6,7-tetrahydro-benzothiazole-2,6-diamine tartrate trihydrate

charcoal

→

(S)-4,5,6,7-tetrahydro-benzothiazole-2,6-diamine

Ausbeute 69.5%

Lösungsmittel

HCl

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigegiving a dark gray solution
2. 2
   workup.ADDITIONTo this was added
3. 3
   FiltrationFiltered the mixture
4. 4
   Waschenwashed with 20 mL H2O
5. 5
   workup.STIRRINGwith stirring
6. 6
   workup.ADDITIONSolid NaOH was added slowly until the pH
7. 7
   TemperaturCooling to room temperature
8. 8
   workup.WAITfollowed by refrigeration for 2 h
9. 9
   Sonstigegave a white ppt
10. 10
    FiltrationFiltered the white ppt
11. 11
    Sonstigedrying oven overnight at 40° C
12. 12
    SonstigeCollected the material

Vorschrift

Dissolved (S)-4,5,6,7-tetrahydro-benzothiazole-2,6-diamine tartrate trihydrate (80.0 g, 214.25 mmol) in 50 mL of 2 M HCl, giving a dark gray solution. To this was added decolorizing charcoal (20 g). The mixture stirred for 30 min. Filtered the mixture and washed with 20 mL H2O. The filtrate was heated at 50° C. with stirring. Solid NaOH was added slowly until the pH was basic. Cooling to room temperature followed by refrigeration for 2 h gave a white ppt. Filtered the white ppt and placed it in a vacuum drying oven overnight at 40° C. Collected the material giving 25.19 g of (S)-4,5,6,7-tetrahydro-benzothiazole-2,6-diamine. 1H NMR showed pure freebase.

Quelle