反应详情

A mixture of 2.28 g. of phenoxyacetic acid, 2.43 g. of 1,1'-carbonyldiimidazole and 50 ml. of tetrahydrofuran was stirred at room temperature for 2 hours, then 3.0 g. of 1H-imidazole-1-propanamine dihydrochloride was added. The reaction mixture was stirred for 18 hours, then heated at reflux temperature for 5 hours, 5 ml. of water was added, the mixture was heated for 30 minutes and then concentrated to remove the tetrahydrofuran. The residue was treated with methylene chloride and 50 ml. of 1N sodium hydroxide and the layers separated. The organic layer was washed with water, dried over magnesium sulfate and concentrated. The residue was washed onto a filter with ether, giving the desired product, m.p. 91°-93° C.

1. additionA mixture of 2.28 g
2. temperatureheated
3. temperatureat reflux temperature for 5 hours
4. temperaturethe mixture was heated for 30 minutes
5. concentrationconcentrated
6. customto remove the tetrahydrofuran
7. additionThe residue was treated with methylene chloride and 50 ml
8. customof 1N sodium hydroxide and the layers separated
9. washThe organic layer was washed with water
10. dry with materialdried over magnesium sulfate
11. concentrationconcentrated
12. washThe residue was washed onto
13. filtrationa filter with ether