HRID845245

反应详情

EQUATION

反应方程式

HRID 845245 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A solution of 0.36 g of 4-methoxymethyl-5-morpholinomethyl-beta-carboline-3-carboxylic acid (prepared according to example 4) in 10 ml of absolute dimethylformamide is mixed with 0.2 g of carbonyldiimidazole and stirred for 30 minutes at 60° C. Then 0.4 g of propioamidoxime in 2 ml of DMF is added and the reaction mixture heated to 100° C. for 3 hours. After distilling off of the solvent in a vacuum, the residue is mixed with 20 ml of xylene and refluxed for 3 hours on the water separator, the reaction mixture is filtered hot, the filtrate is concentrated and chromatographed on silica gel. 0.25 g (60%) of oxadiazole derivative is obtained. Melting point 161°-163° C.

WORKUP

后处理

  1. temperaturethe reaction mixture heated to 100° C. for 3 hours
  2. distillationAfter distilling off of the solvent in a vacuum
  3. additionthe residue is mixed with 20 ml of xylene
  4. temperaturerefluxed for 3 hours on the water separator
  5. filtrationthe reaction mixture is filtered hot
  6. concentrationthe filtrate is concentrated
  7. customchromatographed on silica gel