Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | 3-Bromopyridine-4-carboxaldehyde | HCID 2762997 | — |
| Reactant | 2-Chloro-4-(tetramethyl-1,3,2-dioxaborolan-2-yl)benzonitrile | HCID 57926113 | — |
| Catalyst | HCID 178418476 | HCID 178418476 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 86674839 | HCID 86674839 | 70.1% |
Reaction Steps
A mixture of 2-Chloro-4-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-benzonitrile (0.264 g, 1 mmol), 3-bromoisonicotinaldehyde (0.186 g, 1.000 mmol), sodium carbonate (1.000 ml, 2.000 mmol), bis(triphenylphosphine)palladium(II) chloride (0.018 g, 0.025 mmol) in DMF (6 mL, dry) was heated to 120° C. for 3 hrs. After concentration, the residue was dissolved into CH2Cl2-MeOH and mixed with silica gel and concentrated. After flash column (MeOH—CH2Cl2, v/v, 0.5%-1%) yielded 2-chloro-4-(4-formylpyridin-3-yl)benzonitrile (20a) as colorless solid (170 mg) 1H NMR (400.3 MHz, CDCl3): δ 7.63 (d, J=8.0 Hz, 1H), 7.79 (s, 1H), 7.83 (d, J=8.0 Hz, 1H), 8.35 (s, 1H), 9.07 (s, 1H), 9.15 (s, 1H), 10.22 (s, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08519134B2 |
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| Source dataset | uspto-grants-2013_08 |
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| ORD ID | ord-5a79e39b465a448a98b741ff82d6cf36 |
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| Source note | uspto-grants-2013_08 |
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