反応 #55121

反応方程式

hydrochloric acid

2-Chloromethylpyrazine

sodium

cysteamine hydrochloride

→

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

溶媒

ethanol

反応条件

後処理

1. 1
   workup.ADDITIONhad been added gradually at 0°
2. 2
   その他The suspension finally obtained
3. 3
   workup.STIRRINGwas stirred at room temperature overnight
4. 4
   濃縮concentrated under reduced pressure
5. 5
   抽出The dry residue was extracted with ethanol
6. 6
   ろ過the extracts filtered
7. 7
   濃縮concentrated
8. 8
   その他to give the crude product
9. 9
   抽出Extraction with isopropyl alcohol
10. 10
    その他with the removal of some polymeric material
11. 11
    workup.ADDITIONthe addition of ether
12. 12
    その他gave a cream colored solid (3.5 g.), which
13. 13
    その他was recrystallised from ethanol-ether

実験手順

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°.

出典