HRID127275
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
The starting material is prepared as follows: The mixture of 200 g of 3,3-tetramethyleneglutaric anhydride, 57 g of 4-aminopyridine and 1,500 ml of xylene is stirred and refluxed on a water separator for 3 days. After cooling slightly, the xylene solution is decanted from a small amount of oily material, and after cooling in an ice bath, the collected residue dissolved in 1,500 ml of boiling ethanol, the solution cooled to 5°, filtered and the residue dried, to yield the 8-(4-pyridyl)-8-azaspiro[4,5]decan-7,9-dione melting at 208°-211°.
WORKUP
后处理
- customThe starting material is prepared
- temperatureAfter cooling slightly
- customthe xylene solution is decanted from a small amount of oily material
- temperatureafter cooling in an ice bath
- dissolutionthe collected residue dissolved in 1,500 ml of boiling ethanol
- temperaturethe solution cooled to 5°
- filtrationfiltered
- customthe residue dried