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 0.51 g of 4-[(2-methylbenzoyl)amino]benzoyl chloride and 0.36 g of 1,1'-carbonyldiimidazole in 6 ml of tetrahydrofuran is stirred at room temperature for 1 hour. To the reaction mixture is added 0.17 g of 4,5-dihydropyrrolo-[1,2-a]-quinoxaline followed by heating at reflux for 60 hours. The volatiles are concentrated vacuo to a residue which is dissolved in ethyl acetate. The organic layer is washed with 1N HCl, 1M NaHCO3, brine, dried with Na2SO4 and filtered through hydrous magnesium silicate. The volatiles are concentrated in vacuo to a residue which is chromatographed by elution with 1:2 ethyl acetate-hexanes to give 0.14 g of the desired product as a white solid, m.p. 206°-207° C.;
WORKUP
后处理
- temperatureby heating
- temperatureat reflux for 60 hours
- concentrationThe volatiles are concentrated vacuo to a residue which
- dissolutionis dissolved in ethyl acetate
- washThe organic layer is washed with 1N HCl, 1M NaHCO3, brine
- dry with materialdried with Na2SO4
- filtrationfiltered through hydrous magnesium silicate
- concentrationThe volatiles are concentrated in vacuo to a residue which
- customis chromatographed by elution with 1:2 ethyl acetate-hexanes