Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Pivalic acid | HCID 6417 | — |
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 57816297 | HCID 57816297 | — |
| Catalyst | palladium(II) acetate | HCID 167845 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 66797980 | HCID 66797980 | — |
Reaction Steps
50 ml of pivalic acid are added to 15 g of (9,9-diphenyl-9H-fluoren-2-yl)phenylamine (36.6 mmol), 0.9 g of palladium(II)acetate (3.66 mmol) and 0.5 g of potassium carbonate (3.66 mmol), and the mixture is stirred at 120° C. for 9 h. After this time, 0.9 g of palladium(II)acetate (3.66 mmol) is added, and the mixture is stirred at 120° C. for a further 9 h. 200 ml of dichloromethane and 0.1 M Na2CO3 solution are then added. The mixture is partitioned between water and dichloromethane, the aqueous phase is extracted three times with dichloromethane, and the combined organic phases are dried over Na2SO4 and evaporated in a rotary evaporator. The residue is recrystallised from toluene/heptane. The yield is 6 g (14.6 mmol, 40%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09126970B2 |
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| Source dataset | uspto-grants-2015_09 |
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| ORD ID | ord-1f84a011172d4af38cfa245d9bdbc66a |
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| Source note | uspto-grants-2015_09 |
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