Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | (2-(Dimethylamino)ethyl)triphenylphosphonium bromide | HCID 2724136 | — |
| Reactant | 7-(2-Fluoro-4-nitrophenoxy)thieno[3,2-b]pyridine-2-carbaldehyde | HCID 58790381 | — |
| Reactant | Butyllithium | HCID 178418339 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 66649106 | HCID 66649106 | 79.4% |
Reaction Steps
To a solution of (2-(dimethylamino)ethyl)triphenylphosphonium bromide (680 mg, 1.54 mmol) in THF (7.7 mL) was added n-BuLi (2.5M in hexanes, 0.65 mL, 1.62 mmol) dropwise at 0° C., the resulting mixture was warmed to room temperature and stirred for 30 min. 7-(2-fluoro-4-nitrophenoxy)thieno[3,2-b]pyridine-2-carbaldehyde 233 (500 mg, 1.17 mmol) was added in one portion and the mixture was stirred for 2 h. The mixture was poured into water, extracted with EtOAc; the organic phase was extracted with 3% citric acid, the combined aqueous phase was basified to pH˜11 by the addition of 1N NaOH. It was then extracted with EtOAc, dried over anhydrous Na2SO4 and concentrated under reduced pressure affording title compound 234 (360 mg, 0.929 mmol, 78% yield) as a crude mixture that was used in the next step without further purification. MS (m/z): (M+1) 388.1 (100%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08329726B2 |
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| Source dataset | uspto-grants-2012_12 |
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| ORD ID | ord-fd41fcf5e739471c982138746bafc1a1 |
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| Source note | uspto-grants-2012_12 |
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