反应详情

A mixture of 1.22 g. of benzoic acid, 1.62 g. of 1,1'-carbonyldiimidazole and 30 ml. of tetrahydrofuran was stirred for 3 hours, then 1.98 g. of 1H-imidazole-1-propanamine dihydrochloride was added. The reaction mixture was stirred for 18 hours, then heated at reflux for 5 hours, then diluted with 5 ml. of water and heated for an additional 30 minutes. The mixture was concentrated to remove most of the solvent and to the residue was added chloroform and 35 ml. of 1N sodium hydroxide. The layers were separated. The organic layer was washed with water, dried over magnesium sulfate, concentrated and diethyl ether was added, giving the desired product, m.p. 134°-136° C.

1. additionA mixture of 1.22 g
2. temperatureheated
3. temperatureat reflux for 5 hours
4. additiondiluted with 5 ml
5. concentrationThe mixture was concentrated
6. customto remove most of the solvent and to the residue
7. additionwas added chloroform and 35 ml
8. customThe layers were separated
9. washThe organic layer was washed with water
10. dry with materialdried over magnesium sulfate
11. concentrationconcentrated
12. additiondiethyl ether was added