HRID21371

反应详情

EQUATION

反应方程式

HRID 21371 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

8.2 g (0.054 mol) of 4-[(ethylthio)methyl]pyridine are dissolved in 60 ml of acetonitrile and then 9.1 g of methyliodide are added. After 12 hours the reaction mixture is evaporated down in vacuo. The residue is reacted analogously to Example 1 b) with sodium borohydride in methanol and worked up. The crude product obtained is distilled (5.2 g; 56.3% of theory; b.p. 118°-120° C./20 mbar) and then chromatographed on neutral aluminium oxide using chloroform as eluant. 4.4 g of 4-[(ethylthio)methyl]-1-methyl-1,2,3,6-tetrahydropyridine are obtained, which is converted with one equivalent of maleic acid into the maleate (m.p. 102°-105° C., from ethyl acetate).

WORKUP

后处理

  1. customAfter 12 hours the reaction mixture is evaporated down in vacuo
  2. customThe residue is reacted analogously to Example 1 b) with sodium borohydride in methanol
  3. customThe crude product obtained
  4. distillationis distilled (5.2 g; 56.3% of theory; b.p. 118°-120° C./20 mbar)
  5. customchromatographed on neutral aluminium oxide