Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 68688462 | HCID 68688462 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 68690484 | HCID 68690484 | 86.3% |
Reaction Steps
A solution of 2,2′,6′-trimethyl-biphenyl-4-carboxylic acid methyl ester of Step A (18.5 g, 75.4 mmole) in tetrahydrofuran was treated with 1 N sodium hydroxide (250 mL) and heated at 90° C. for 20 hours. The mixture was acidified to pH ˜1 with concentrated hydrochloric acid, extracted with dichloromethane, dried over anhydrous magnesium sulfate, and concentrated to give the title compound as a white powder (15.63 g). Recrystallization from aqueous ethanol provided white plates, m.p. 172-173° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07687623B2 |
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| Source dataset | uspto-grants-2010_03 |
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| ORD ID | ord-39ebc9013a684d3498f326184e4eb8c1 |
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| Source note | uspto-grants-2010_03 |
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