HuagongsheHuagongshe Chemistry Print Report · For research reference only
Benzene → 2-(4,4'-Difluorobenzhydrylidene)-1,3,5-trithiane
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Benzene | HCID 241 | — |
| Reactant | p-Toluenesulfonic acid | HCID 6101 | — |
| Reactant | 2-{Bis(4-fluorophenyl)hydroxymethyl}-1,3,5-trithiane | HCID 14329258 | — |
| Solvent | Cyclohexane | HCID 8078 | — |
| Product | 2-(4,4'-Difluorobenzhydrylidene)-1,3,5-trithiane | HCID 14329284 | 89.5% |
Reaction Steps
A mixture of 2.0 g of 2-{bis(4-fluorophenyl)hydroxymetyl}-1,3,5-trithiane, 0.2 g of p-toluenesulfonic acid and 50 ml of benzene was refluxed with heating for 15 minutes by means of a Dean-Stark reflux condenser. After being cooled, the mixture was extracted with ethyl acetate and the extract was washed with a saturated aqueous sodium hydrogencarbonate solution. The washed extract was dried over anhydrous magnesium sulfate and the solvent was removed by distillation under reduced pressure to obtain a material, which was recrysallized from cyclohexane to give 1.7 g of the desired compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04816475 |
| Source dataset | uspto-grants-1989_03 |
| ORD ID | ord-0f0bcebbd6df4aafbc84d24ac2015dc3 |
| Source note | uspto-grants-1989_03 |