HRID1886356
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
A mixture of 3.76 parts of 4-(1H-imidazol-1-ylmethyl)-1,2-benzenediamine, 4.5 parts of diphenylethanedione and 80 parts of ethanol was stirred for 4 hours at reflux temperature. The reaction mixture was concentrated and the concentrate was purified by column chromatography over silica gel using a mixture of trichloromethane and methanol (95:5 by volume) as eluent. The pure fractions were collected and the eluent was evaporated. The residue was crystallized from a mixture of 1,1'-oxybisethane and ethanol. The product was filtered off and dried, yielding 4 parts (55%) of 6-(1H-imidazol-1-ylmethyl)-2,3-diphenylquinoxaline; mp. 159.3° C. (comp. 8).
WORKUP
后处理
- temperatureat reflux temperature
- concentrationThe reaction mixture was concentrated
- customthe concentrate was purified by column chromatography over silica gel using
- additiona mixture of trichloromethane and methanol (95:5 by volume) as eluent
- customThe pure fractions were collected
- customthe eluent was evaporated
- customThe residue was crystallized from a mixture of 1,1'-oxybisethane and ethanol
- filtrationThe product was filtered off
- customdried