HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Carbonate → 3,6-DI-Tert-butyl-2,7-diphenyl-9H-fluorene
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | Phenylboronic Acid | HCID 66827 | — |
| Reactant | 2,7-Dibromo-3,6-DI-tert-butyl-9H-fluorene | HCID 13547542 | — |
| Catalyst | HCID 178418397 | HCID 178418397 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | 3,6-DI-Tert-butyl-2,7-diphenyl-9H-fluorene | HCID 21982695 | 179.4% |
Reaction Steps
To a mixture of 2,7-dibromo-3,6-di-t-butylfluorene (0.96 g, 2.20 mmol) and Pd(PPh3)4 (260 mg, 0.22 mmol) in toluene (50 ml) was added a solution of phenylboronic acid (0.81 g, 6.63 mmol) in EtOH (10 ml) and a solution of Na2CO3 (1.5 g) in water (10 ml). The reaction mixture was stirred for 6 hours under reflux. The reaction mixture was quenched with water, extracted with ether, dried over MgSO4, and evaporated under vacuum to afford the residue which was purified by column chromatography (silica gel, hexane/CH2Cl2=5/1) to produce 2,7-diphenyl-3,6-di-t-butyl-fluorene (0.85 g, ˜90%). 1H NMR (CDCl3): δ 7.96 and 7.15 (each s, 2H, 1,8- and 4,5-H (Flu), 7.33 (m, 10H, Ph), 3.77 (s, 2H, H9), 1.27 (s, 18H, t-Bu).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08093418B2 |
| Source dataset | uspto-grants-2012_01 |
| ORD ID | ord-0e3c1622f4754cbba46c36b1bb5dcc54 |
| Source note | uspto-grants-2012_01 |