反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- additionhad been added gradually at 0°
- customThe suspension finally obtained
- stirringwas stirred at room temperature overnight
- concentrationconcentrated under reduced pressure
- extractionThe dry residue was extracted with ethanol
- filtrationthe extracts filtered
- concentrationconcentrated
- customto give the crude product
- extractionExtraction with isopropyl alcohol
- customwith the removal of some polymeric material
- additionthe addition of ether
- customgave a cream colored solid (3.5 g.), which
- customwas recrystallised from ethanol-ether