HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Hydroxybenzoic Acid → 2,7-Bis(4-hydroxybenzoyloxy)-9-methylfluorene
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Hydroxybenzoic Acid | HCID 135 | — |
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | Boric Acid | HCID 7628 | — |
| Reactant | 9-methyl-9H-fluorene-2,7-diol | HCID 21960627 | — |
| Solvent | O-Xylene | HCID 7237 | — |
| Product | 2,7-Bis(4-hydroxybenzoyloxy)-9-methylfluorene | HCID 59434463 | 70% |
Reaction Steps
In a nitrogen atmosphere, concentrated sulfuric acid (0.2 mL) was added to a mixture of 4-hydroxybenzoic acid (13.0 g), 2,7-dihydroxy-9-methylfluorene (10.0 g), boric acid (0.3 g) and xylene (120 mL), and the mixture was heated under reflux for 6 hours while removing water. A solid matter thus deposited was collected by filtration under reduced pressure, and rinsed with toluene. The solid matter was recrystallized from a mixed solvent of ethanol (75 mL) and acetone (75 mL) to provide 2,7-bis(4-hydroxybenzoyloxy)-9-methylfluorene (compound [H1]) (14.9 g) in the form of pale rose crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07985455B2 |
| Source dataset | uspto-grants-2011_07 |
| ORD ID | ord-13e26a18a2c44b1a91829a7d0d1611b0 |
| Source note | uspto-grants-2011_07 |