Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Npc316347 | HCID 3280088 | — |
| Reactant | 5-Bromo-2-fluoro-6'-methoxy-[3,4]bipyridinyl-3'-ylamine | HCID 58266519 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 58266529 | HCID 58266529 | 47% |
Reaction Steps
A 1N solution of bis(trimethylsilyl)amide in THF (6.81 mL, 6.81 mmol) was added dropwise to a solution of 5-bromo-2-fluoro-6′-methoxy-[3,4′]bipyridinyl-3′-ylamine (203 mg, 0.681 mmol) in THF (12.0 mL). The reaction mixture was stirred for 30 minutes at ambient temperature, diluted with water, and extracted into ethyl acetate. The organic phase was dried over sodium sulfate, filtered, and concentrated in vacuo. The crude residue was dissolved in ethyl acetate and methanol, absorbed onto silica gel, and purified by flash chromatography (silica, 12 g column, ISCO, 0-100% ethyl acetate in hexanes) to provide the title compound as an orange-tan solid (89.0 mg, 47%). 1H NMR (DMSO-D6, 400 MHz): 12.44-12.12 (m, 1H), 7.79 (d, J=2.6 Hz, 1H), 7.66 (d, J=3.5 Hz, 2H), 6.56 (s, 1H), 3.75 (s, 3H). LCMS (Method B): RT=1.83 min, M+H+=278/280.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09216980B2 |
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| Source dataset | uspto-grants-2015_12 |
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| ORD ID | ord-166abb756ab246abbc547ab26915e1c8 |
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| Source note | uspto-grants-2015_12 |
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