反应详情

温度

10 °C

Chlorosulfonic acid (500 g.) was taken in a three neck round bottom flask equipped with a guard tube and cooled it to 10° C. N-acetyl 2-toluidine (100 g.) was added in small portions maintaining temperature below 10° C. After complete addition of 2-methoxy acetanilide cooling is removed and reaction was brought to 25° C. Reaction mixture was stirred at 25° C. for further 24 hours. After the completion of reaction (TLC), the reaction mixture was poured on ice-water, and the resulting slurry was filtered on buchner funnel. Solid cake on funnel was washed with 500 mL of water and the resulting solid was dried on phosphorus pentoxide in a desiccator to obtain 113.5 grams off white solid. It was found to contain a mixture of two isomers as confirmed from NMR and HPLC; however the desired isomer was obtained by partial crystallization using benzene and used for further experimentation, after the thorough carectorisation.

1. customequipped with a guard tube
2. temperaturemaintaining temperature below 10° C
3. customis removed
4. customreaction
5. customwas brought to 25° C
6. customReaction mixture
7. customAfter the completion of reaction (TLC)
8. additionthe reaction mixture was poured on ice-water
9. filtrationthe resulting slurry was filtered on buchner funnel
10. washSolid cake on funnel was washed with 500 mL of water
11. customthe resulting solid was dried on phosphorus pentoxide in a desiccator
12. customto obtain 113.5 grams off white solid
13. additiona mixture of two isomers
14. customhowever the desired isomer was obtained by partial crystallization