HRID345444

反应详情

EQUATION

反应方程式

HRID 345444 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 4-chloropyridine hydrochloride (7.50 g), 4-hydroxypiperidine (5.06 g) and sodium bicarbonate (10.1 g) in isoamyl alcohol (60 ml) was heated under reflux with stirring for 60 hours and then evaporated. The residue was extracted several times with a boiling mixture of ethyl acetate/methanol (10:1) and the combined extracts were filtered and evaporated. The residue was sublimed at 120°-150° and 0.2 mm pressure to give the pure product, (7.30 g), m.p. 155°-156°.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux
  3. customevaporated
  4. extractionThe residue was extracted several times
  5. additionwith a boiling mixture of ethyl acetate/methanol (10:1)
  6. filtrationthe combined extracts were filtered
  7. customevaporated
  8. customwas sublimed at 120°-150°
  9. custom0.2 mm pressure to give the pure product, (7.30 g), m.p. 155°-156°