反应详情

温度

60 °C

Methyl 4-[2-[N-(4-chlorophenyl)amino]ethoxy]benzoate (0.4 g) was suspended in methanol (20 ml), and thereto a solution of sodium hydroxide (0.16 g) in water (5 ml) was added, and the mixture was heated with stirring at 60° C. for 3 hours. The reaction mixture was cooled, and neutralized with hydrochloric acid and concentrated under reduced pressure. After adding water thereto, the resulting residue was crushed, then, collected by filtration to give crude crystal. An equivalent amount of hydrochloric acid was added to the crude crystal in methanol, and the mixture was dried under reduced pressure to give a salt. The salt was suspended in a mixed solvent of methanol and ether, and collected by filtration to give the desired product (0.31 g). mp. 190°-193° C.

1. temperaturethe mixture was heated
2. temperatureThe reaction mixture was cooled
3. concentrationconcentrated under reduced pressure
4. additionAfter adding water
5. customthe resulting residue was crushed
6. filtrationcollected by filtration
7. customto give crude crystal
8. customthe mixture was dried under reduced pressure
9. customto give a salt
10. filtrationcollected by filtration