HRID26843

反应详情

EQUATION

反应方程式

HRID 26843 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

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°.

WORKUP

后处理

  1. additionhad been added gradually at 0°
  2. customThe suspension finally obtained
  3. stirringwas stirred at room temperature overnight
  4. concentrationconcentrated under reduced pressure
  5. extractionThe dry residue was extracted with ethanol
  6. filtrationthe extracts filtered
  7. concentrationconcentrated
  8. customto give the crude product
  9. extractionExtraction with isopropyl alcohol
  10. customwith the removal of some polymeric material
  11. additionthe addition of ether
  12. customgave a cream colored solid (3.5 g.), which
  13. customwas recrystallised from ethanol-ether