تفاعل #55121

معادلة التفاعل

hydrochloric acid

2-Chloromethylpyrazine

sodium

cysteamine hydrochloride

→

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

المذيبات

ethanol

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONhad been added gradually at 0°
2. 2
   أخرىThe suspension finally obtained
3. 3
   workup.STIRRINGwas stirred at room temperature overnight
4. 4
   تركيزconcentrated under reduced pressure
5. 5
   استخلاصThe dry residue was extracted with ethanol
6. 6
   ترشيحthe extracts filtered
7. 7
   تركيزconcentrated
8. 8
   أخرىto give the crude product
9. 9
   استخلاصExtraction with isopropyl alcohol
10. 10
    أخرىwith the removal of some polymeric material
11. 11
    workup.ADDITIONthe addition of ether
12. 12
    أخرىgave a cream colored solid (3.5 g.), which
13. 13
    أخرىwas recrystallised from ethanol-ether

الإجراء التجريبي

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°.

المصدر