反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
1-(1-Ethylpropyl)-8-methoxy-4-oxo-4,5-dihydroimidazo[1,5-a]-quinoxaline-7-carboxyic acid as synthesized in above Example 32, 329 mg, N,N-diimethylformamide 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
- additionwere mixed
- stirring' stirring
- extractionextracted with ethyl acetate
- washwashed with saturated saline
- dry with materialThe extract was dried over anhydrous sodium sulfate
- distillationfrom which the solvent was distilled off
- additionTo the residue tert-butyl methyl ether was added
- temperatureheated
- stirringunder stirring
- filtrationthe precipitate was recovered by filtration
- washby washing with tert-butyl methyl ether
- customThe product was dried
- customair (40° C.)