HRID35334
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
A mixture of 23.8 parts of N-(2,6-dichlorophenyl)hexahydro-3,3-dimethyl-1-oxoimidazo[1,5-a]pyrazine-7(8H)-acetamide and 256 parts of a hydrochloric acid solution 0.5N was stirred and refluxed for 2 hours. The reaction mixture was cooled overnight to room temperature, alkalized and salted out with sodium carbonate. The product was extracted with trichloromethane. The extract was filtered and the filtrate was dried, filtered and evaporated. The residue was crystallized from acetonitrile, yielding 13.6 parts (64%) of 3-(aminocarbonyl)-N-(2,6-dichlorophenyl)-1-piperazineacetamide; mp. 180.4°-182.8° C. (intermediate 125).
WORKUP
后处理
- temperaturerefluxed for 2 hours
- temperatureThe reaction mixture was cooled overnight to room temperature
- extractionThe product was extracted with trichloromethane
- filtrationThe extract was filtered
- customthe filtrate was dried
- filtrationfiltered
- customevaporated
- customThe residue was crystallized from acetonitrile