반응 #55121

반응 방정식

hydrochloric acid

2-Chloromethylpyrazine

sodium

cysteamine hydrochloride

→

2-[(2-aminoethyl)thiomethyl]pyrazine hydrochloride

용매

ethanol

반응 조건

후처리

1. 1
   workup.ADDITIONhad been added gradually at 0°
2. 2
   기타The suspension finally obtained
3. 3
   workup.STIRRINGwas stirred at room temperature overnight
4. 4
   농축concentrated under reduced pressure
5. 5
   추출The dry residue was extracted with ethanol
6. 6
   여과the extracts filtered
7. 7
   농축concentrated
8. 8
   기타to give the crude product
9. 9
   추출Extraction with isopropyl alcohol
10. 10
    기타with the removal of some polymeric material
11. 11
    workup.ADDITIONthe addition of ether
12. 12
    기타gave a cream colored solid (3.5 g.), which
13. 13
    기타was recrystallised from ethanol-ether

실험 절차

2-Chloromethylpyrazine (6.4 g.) was added over 20 minutes to a solution freshly prepared from sodium (0.23 g.) in ethanol (50 ml.) to which cysteamine hydrochloride (5.7 g.) had been added gradually at 0° and stirred at this temperature for 2 hours. The suspension finally obtained was stirred at room temperature overnight, acidified with hydrochloric acid (pH 5) and concentrated under reduced pressure. The dry residue was extracted with ethanol and the extracts filtered and concentrated to give the crude product. Extraction with isopropyl alcohol, with the removal of some polymeric material and the addition of ether gave a cream colored solid (3.5 g.), which was recrystallised from ethanol-ether to furnish 2-[(2-aminoethyl)thiomethyl]pyrazine hydrochloride, m.p. 144°-146°.

출처