HRID345444
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
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
- temperaturewas heated
- temperatureunder reflux
- customevaporated
- extractionThe residue was extracted several times
- additionwith a boiling mixture of ethyl acetate/methanol (10:1)
- filtrationthe combined extracts were filtered
- customevaporated
- customwas sublimed at 120°-150°
- custom0.2 mm pressure to give the pure product, (7.30 g), m.p. 155°-156°