반응 #505530

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

charcoal

→

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

수율 69.5%

용매

HCl

반응 조건

후처리

1. 1
   기타giving a dark gray solution
2. 2
   workup.ADDITIONTo this was added
3. 3
   여과Filtered the mixture
4. 4
   세척washed with 20 mL H2O
5. 5
   workup.STIRRINGwith stirring
6. 6
   workup.ADDITIONSolid NaOH was added slowly until the pH
7. 7
   온도Cooling to room temperature
8. 8
   workup.WAITfollowed by refrigeration for 2 h
9. 9
   기타gave a white ppt
10. 10
    여과Filtered the white ppt
11. 11
    기타drying oven overnight at 40° C
12. 12
    기타Collected the material

실험 절차

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.

출처