反应详情

A mixture of 9.61 g of 3-p-chlorobenzoyl phenyl acetonitrile, 75 cc of water, 75 cc of acetic acid and 75 cc of sulfuric acid was refluxed with stirring for 21/2 hours and then cooled and iced for 1 hour. The mixture was vacuum filtered and the precipitate was empasted with water and taken up in 50 cc of a 10% aqueous sodium carbonate solution. The solution was filtered and the filter was washed with water. The pH of the filtrate was adjusted to 5-6 by addition of acetic acid and after being iced for 30 minutes, the mixture was vacuum filtered. The recovered precipitate was washed with water and dried under reduced pressure. The residue was dissolved in 50 cc of refluxing toluene and the solution was treated with activated carbon and filtered. The filter was washed with boiling toluene. The filtrate was cooled and iced for 1 hour and then vacuum filtered. The recovered precipitate was empasted with iced toluene and dried under reduced pressure to obtain 8.37 g of 3-p-chlorobenzoyl phenyl-acetic acid melting at 148° C.

1. temperaturewas refluxed
2. temperaturecooled
3. waiticed for 1 hour
4. filtrationfiltered
5. filtrationThe solution was filtered
6. washthe filter was washed with water
7. additionThe pH of the filtrate was adjusted to 5-6 by addition of acetic acid
8. waitafter being iced for 30 minutes
9. filtrationfiltered
10. washThe recovered precipitate was washed with water
11. customdried under reduced pressure
12. dissolutionThe residue was dissolved in 50 cc of refluxing toluene
13. additionthe solution was treated with activated carbon
14. filtrationfiltered
15. washThe filter was washed with boiling toluene
16. temperatureThe filtrate was cooled
17. waiticed for 1 hour
18. filtrationvacuum filtered
19. customdried under reduced pressure