Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Benzoic Acid | HCID 243 | — |
| Reactant | HCID 67506337 | HCID 67506337 | — |
| Reactant | Phosphorus Pentoxide-Methanesulfonic Acid | HCID 86584057 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 67506256 | HCID 67506256 | 81% |
Reaction Steps
In a 500 mL recovery flask, 44.9 g of 2,7-di(1-adamantyl)-fluorenone obtained in the same manner as in Synthesis example 7 (100 mmol), 36.6 g of benzoic acid (300 mmol), 203 mL of Eaton's reagent (7.7 wt % methanesulfonic acid solution of diphosphorus pentoxide) and a stirrer were charged and agitated at 150° C. for 12 hours under a nitrogen atmosphere. After reaction solution reached room temperature, mL of ion-exchange water was added slowly. An aqueous layer was separated and removed therefrom. Then, solvent was removed from the reaction solution under reduced pressure. Solid thus obtained was purified by column chromatography, thus obtaining 54.7 g of 2,7-di(1-adamantyl)-fluorene-9,9-bisbenzoic acid (81 mmol; yield: 81%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US07863347B2 |
|---|
| Source dataset | uspto-grants-2011_01 |
|---|
| ORD ID | ord-aa19830375ae498f861f99381caea4dc |
|---|
| Source note | uspto-grants-2011_01 |
|---|