HRID2068941

反应详情

EQUATION

反应方程式

HRID 2068941 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1-(1-Ethylpropyl)-8-methoxy-4-oxo-4,5-dihydroimidazo[1,5-a]-quinoxaline-7-carboxylic acid as synthesized in above Example 32, 329 mg, N,N-dimethylformamide 5 mL and 1,1′-carbonyldiimidazole 275 mg were mixed and stirred for an hour at room temperature in nitrogen atmosphere. Dimethylamine hydrochloride 816 mg was added, followed by 5.5 hours' stirring. The reaction mixture was diluted with water, extracted with ethyl acetate and washed with saturated saline. The extract was dried over anhydrous sodium sulfate, and from which the solvent was distilled off. To the residue tert-butyl methyl ether was added, heated under stirring, and the precipitate was recovered by filtration, followed by washing with tert-butyl methyl ether. The product was dried in flowing air (40° C.) to provide 223 mg of the title compound.

WORKUP

后处理

  1. additionwere mixed
  2. stirring' stirring
  3. extractionextracted with ethyl acetate
  4. washwashed with saturated saline
  5. dry with materialThe extract was dried over anhydrous sodium sulfate
  6. distillationfrom which the solvent was distilled off
  7. additionTo the residue tert-butyl methyl ether was added
  8. temperatureheated
  9. stirringunder stirring
  10. filtrationthe precipitate was recovered by filtration
  11. washby washing with tert-butyl methyl ether
  12. customThe product was dried
  13. customair (40° C.)