反应详情

5 g of [Benzyl-(2-hydroxyethyl)-amino]-(4-fluorophenyl)-acetonitrile of Formula XI and 15 ml of dimethylsulfoxide (DMSO) were charged in a clean and dry 4 neck round bottom flask followed by stirring for about 20 minutes. 3.8 g. of potassium carbonate was charged to the above reaction solution followed by addition of 7 ml of 50% hydrogen peroxide over about 30 minutes. The resultant reaction solution was stirred for about 2 hours, after completion of the reaction, reaction was quenched by adding 50 ml of water over about 30 minutes. The reaction suspension was stirred for about 1 hour. Separated solid was filtered and the solid was washed with 10 ml of water. Wet cake obtained and 50 ml of petroleum ether were charged in a clean and dry 4neck round bottom flask followed by stirring for about 15 minutes. The solid was filtered and the solid was dried at about 30° C. for about 5 hours to yield 3.8 g of the title compound.

1. customdry 4 neck round bottom flask
2. additionof potassium carbonate was charged to the above reaction solution
3. additionfollowed by addition of 7 ml of 50% hydrogen peroxide over about 30 minutes
4. customThe resultant reaction solution
5. stirringwas stirred for about 2 hours
6. customafter completion of the reaction, reaction
7. customwas quenched
8. additionby adding 50 ml of water over about 30 minutes
9. stirringThe reaction suspension was stirred for about 1 hour
10. customSeparated solid
11. filtrationwas filtered
12. washthe solid was washed with 10 ml of water
13. customWet cake obtained
14. customdry
15. customround bottom flask followed
16. stirringby stirring for about 15 minutes
17. filtrationThe solid was filtered
18. customthe solid was dried at about 30° C. for about 5 hours