반응 #564148

반응 방정식

sodium borohydride

hydrochloric acid

2,6-diamino- 4,5,6,7-tetrahydro-benzthiazole

n- butanal

→

2-Amino-6-n-butylamino-4,5,6,7-tetrahydro-benzthiazole-dihydrochloride

용매

water

dimethylformamide

반응 조건

후처리

1. 1
   온도After cooling
2. 2
   온도heated to 50° C. for 30 minutes
3. 3
   온도Whilst cooling with ice
4. 4
   기타is obtained
5. 5
   추출The aqueous solution is extracted with ethylacetate
6. 6
   workup.ADDITIONThe aqueous phase is mixed with potassium carbonate until an alkaline reaction
7. 7
   기타is obtained
8. 8
   추출extracted with ethyl acetate
9. 9
   기타The organic phase is dried
10. 10
    농축concentrated
11. 11
    기타The compound crystallizes out when ethereal hydrochloric acid
12. 12
    workup.ADDITIONis added

실험 절차

To a solution of 3.4 g (0.02 Mol) of 2,6-diamino- 4,5,6,7-tetrahydro-benzthiazole in 34 ml of dimethylformamide are added 1.8 g (0.022 Mol) of n- butanal and the mixture is heated to 50° C. for 1 hour. After cooling, the reaction solution is mixed with 0.8 g (0.02 Mol) of sodium borohydride and heated to 50° C. for 30 minutes. The solvent is largely eliminated in vacuo. Whilst cooling with ice, the residue is mixed with 20 ml of water and 2N hydrochloric acid until a pH of 1 is obtained. The aqueous solution is extracted with ethylacetate and the organic phase discarded. The aqueous phase is mixed with potassium carbonate until an alkaline reaction is obtained and then extracted with ethyl acetate. The organic phase is dried and concentrated. The compound crystallizes out when ethereal hydrochloric acid is added.

출처