HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dicyclohexylcarbodiimide → Pentafluorophenyl 4'-Octyloxy-biphenyl-4-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dicyclohexylcarbodiimide | HCID 10868 | — |
| Reactant | Pentafluorophenol | HCID 13041 | — |
| Reactant | 4'-(Octyloxy)-[1,1'-biphenyl]-4-carboxylic acid | HCID 2802556 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | Pentafluorophenyl 4'-Octyloxy-biphenyl-4-carboxylate | HCID 15548597 | 96.6% |
Reaction Steps
100 g of 4-octyloxybiphenyl-4′carboxylic acid and 62 g of pentafluorophenol are introduced into 1 liter of dichloromethane. Agitation is carried out for 15 minutes and 69.6 g of N,N′-dicyclohexylcarbodiimide in solution in 500 ml of dichloromethane is added over 15 minutes. The dark beige suspension is agitated for 20 hours at ambient temperature. The dicyclohexylurea is filtered and the filtrate is concentrated. Distillation to constant volume is carried out by the regular addition of ethanol up to the vapour temperature of 74° C. The reaction medium is cooled down to ambient temperature, followed by agitating for one hour, filtering then washing with ethanol. After drying, 145.7 g of sought product is obtained in the form of crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07148322B2 |
| Source dataset | uspto-grants-2006_12 |
| ORD ID | ord-9b1f9c04c5f54f36a20ecb00750cedbd |
| Source note | uspto-grants-2006_12 |