Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 58074814 | HCID 58074814 | — |
| Reactant | HCID 131733111 | HCID 131733111 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 89751845 | HCID 89751845 | 32% |
Reaction Steps
To a solution of 1,1′-(2,2′-dihydroxy-[1,1′-biphenyl]-4,4′-diyl)-diethanone (0.2 g, 0.74 mmol) (synthesized according to WO 2010/111673) in anhydrous DMF (10 mL), NaOH (0.08 g, 1.85 mmol) and 2,2-dimethylpropane-1,3-diyl-bis-(4-methylbenzenesulfonate) (0.37 g, 0.89 mmol) (synthesized according to US 2005/0113374) were added successively and the suspension was stirred at 150° C. for 20 h under nitrogen atmosphere. The reaction mixture was brought to room temperature, crushed ice was added and stirred vigorously for 15 min. The contents were extracted with ethyl acetate. The organic layer was washed with brine, dried over sodium sulfate and purified by flash column chromatography (20% Ethyl acetate-Hexane) to yield a white solid (0.08 g, 32%). m/z 339.3 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09073943B2 |
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| Source dataset | uspto-grants-2015_07 |
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| ORD ID | ord-aebbc88ab23b4bd28201a2f8e8f629bb |
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| Source note | uspto-grants-2015_07 |
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