反应详情

Toluene (1900 ml) was stirred in a round-bottom flask (5 l) using a water separator. (4-Chlorophenyl)(4-nitrophenyl)methanone (250 g) was added portionwise. p-Toluenesulfonic acid (54.5 g) was added portionwise. Ethylene glycol (237.5 g) was poured out into the mixture. The mixture was stirred and refluxed for 48 hours. The solvent was evaporated. The residue was dissolved into ethyl acetate (5 l) and washed twice with a K2CO3 10% solution. The organic layer was separated, dried, filtered and the solvent was evaporated. The residue was stirred in DIPE, filtered off and dried (vacuum, 40° C., 24 hours), yielding 265 g (91%) of 2-(4-chlorophenyl)-2-(4-nitrophenyl)-1,3-dioxolane (interm. 5-a).

1. temperaturerefluxed for 48 hours
2. customThe solvent was evaporated
3. dissolutionThe residue was dissolved into ethyl acetate (5 l)
4. washwashed twice with a K2CO3 10% solution
5. customThe organic layer was separated
6. customdried
7. filtrationfiltered
8. customthe solvent was evaporated
9. stirringThe residue was stirred in DIPE
10. filtrationfiltered off
11. customdried (vacuum, 40° C., 24 hours)