反应详情

温度

25 °C

To a mixture of 2-aminomethyl-4-benzylmorpholine (3.1 g), 2-acetoxy-4-acetylamino-5-chlorobenzoic acid (4.0 g), and dichloromethane (40 ml) is added 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (2.9 g), and the mixture is stirred at 25° C. for 4 hours. The reaction mixture is washed successively with water and saturated aqueous sodium chloride solution, dried over magnesium sulfate, and evaporated under reduced pressure. The residue is dissolved in ethanol (80 ml), and 10% hydrochloric acid (30 ml) is added. The mixture is refluxed with stirring for 2 hours and concentrated under reduced pressure. The residue is neutralized with aqueous sodium bicarbonate solution and extracted with chloroform. The organic layer is washed successively with water and saturated aqueous sodium chloride solution, dried over magnesium sulfate, and evaporated under reduced pressure. The residue is recrystallized from isopropyl alcohol to give the monohydrate of the title compound (3.0 g), mp 153°-155° C.

1. washThe reaction mixture is washed successively with water and saturated aqueous sodium chloride solution
2. dry with materialdried over magnesium sulfate
3. customevaporated under reduced pressure
4. dissolutionThe residue is dissolved in ethanol (80 ml)
5. addition10% hydrochloric acid (30 ml) is added
6. temperatureThe mixture is refluxed
7. stirringwith stirring for 2 hours
8. concentrationconcentrated under reduced pressure
9. extractionextracted with chloroform
10. washThe organic layer is washed successively with water and saturated aqueous sodium chloride solution
11. dry with materialdried over magnesium sulfate
12. customevaporated under reduced pressure
13. customThe residue is recrystallized from isopropyl alcohol