HRID656478

反应详情

EQUATION

反应方程式

HRID 656478 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

Sodium hydride (22 mmol) washed with pentane is admixed under argon with 20 ml of dimethyl sulphoxide. The mixture is heated at 60° C. for an hour and then diluted with 5 ml of tetrahydrofuran. The mixture is cooled to 0° C. and a solution of 21 mmol of trimethyl-sulphonium iodide in 5 ml of N,N-dimethylformamide is added at 0° C., after which the mixture is stirred for 10 minutes. A solution of 20 mmol of 6,7-dihydro-5H-imidazo[1,5-a]pyridin-8-one [426219-51-4] in 5 ml of N,N-dimethylformamide is added and the reaction mixture is stirred at 60° C. for 18 hours. The reaction mixture is poured into cold brine and extracted with tert-butyl methyl ether. The combined organic phases are washed with brine, dried with sodium sulphate and evaporated. From the residue the title compound is identified by means of flash chromatography (SiO2 60 F) on the basis of the Rf value.

WORKUP

后处理

  1. temperatureThe mixture is cooled to 0° C.
  2. stirringthe reaction mixture is stirred at 60° C. for 18 hours
  3. extractionextracted with tert-butyl methyl ether
  4. washThe combined organic phases are washed with brine
  5. dry with materialdried with sodium sulphate
  6. customevaporated