HRID127275

反应详情

EQUATION

反应方程式

HRID 127275 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customThe starting material is prepared
  2. temperatureAfter cooling slightly
  3. customthe xylene solution is decanted from a small amount of oily material
  4. temperatureafter cooling in an ice bath
  5. dissolutionthe collected residue dissolved in 1,500 ml of boiling ethanol
  6. temperaturethe solution cooled to 5°
  7. filtrationfiltered
  8. customthe residue dried