HRID1415155

反应详情

EQUATION

反应方程式

HRID 1415155 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

A mixture of 5.69 parts of 2-phenyl-(3-pyridyl)-4-(2-azabicyclo[2.2.2]oct-2-yl)butyronitrile, 1.67 parts of sodium azide, 1.38 parts of ammonium chloride and 0.025 parts of lithium chloride in 30 parts by volume of dimethylformamide was stirred for 12 hours under nitrogen at 120° C. After the reaction time was completed, the material was cooled and filtered. The collected precipitate was washed with dimethylformamide and water. The precipitate was then dissolved in 100 parts by volume of 0.2N NaOH. The resultant solution was filtered. The filtrates were neutralized with dilute hydrochloric acid. The product which separated was recrystallized from ethanol. The procedure afforded 5-[1-phenyl-1-(3-pyridyl)-3-(2-azabicyclo[2.2.2]oct-2-yl)propyl]-1H-tetrazole.

WORKUP

后处理

  1. temperaturethe material was cooled
  2. filtrationfiltered
  3. washThe collected precipitate was washed with dimethylformamide and water
  4. dissolutionThe precipitate was then dissolved in 100 parts by volume of 0.2N NaOH
  5. filtrationThe resultant solution was filtered
  6. customThe product which separated
  7. customwas recrystallized from ethanol