反应详情

1.2 Grams of 2-amino-3-(2-quinolon-3-yl)propionic acid and 0.8 ml of triethylamine were suspended in 10 ml of tetrahydrofuran, then under stirring condition at a room temperature, a solution containing 1.0 g of diethyl chlorophosphate in 10 ml of tetrahydrofuran was added dropwise thereto, and the reaction mixture was stirred at a room temperature for 3 hours. To this reaction mixture was added a solution containing 1.0 g of p-chlorobenzoic acid in 10 ml of tetrahydrofuran dropwise and the whole reaction mixture was further stirred at a room temperature for 10 hours. After completion of the reaction, the crystals precipitated were removed by filtration, the filtrate was concentrated and to the residue was poured a saturated sodium hydrogencarbonate aqueous solution, then extracted with chloroform. The organic layer was washed with water and a saturated sodium chloride aqueous solution and dried with sodium sulfare. The solvent was removed by distillation and the residue was recrystallized from ethanol-water to obtain 0.9 g of 2-(4-chlorobenzoylamino)-3-(2-quinolon-3-yl)propionic acid in the form of white powder product.

1. additionwas added dropwise
2. stirringthe reaction mixture was stirred at a room temperature for 3 hours
3. additionTo this reaction mixture was added a solution
4. customthe whole reaction mixture
5. stirringwas further stirred at a room temperature for 10 hours
6. customAfter completion of the reaction
7. customthe crystals precipitated
8. customwere removed by filtration
9. concentrationthe filtrate was concentrated and to the residue
10. additionwas poured a saturated sodium hydrogencarbonate aqueous solution
11. extractionextracted with chloroform
12. washThe organic layer was washed with water
13. dry with materiala saturated sodium chloride aqueous solution and dried with sodium sulfare
14. customThe solvent was removed by distillation
15. customthe residue was recrystallized from ethanol-water