HuagongsheHuagongshe Chemistry Print Report · For research reference only
Allyltributylstannane → HCID 22961885, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Allyltributylstannane | HCID 90628 | — |
| Reactant | HCID 22872668 | HCID 22872668 | — |
| Catalyst | HCID 178418397 | HCID 178418397 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 22961885 | HCID 22961885 | 110.3% |
Reaction Steps
3-(1-BOC-2-(S)-pyrrolidinylmethoxy)-5-bromo-6-chloropyridine (2.0 g, 5.14 mmol) in toluene (15 mL) was added tetrakis(triphenylphosphine)palladium (15 mg) and allyltributyltin (3.2 mL, 10.2 mmol). The mixture was stirred and refluxed for 16 h. Solvent was evaporated and the residue was chromatographed (silica gel; hexane/EtOAc, 5:1 to 1:1) to afford an oil (2.0 g, 100%): 1H NMR (CDCl3, 300 MHz) δ 1.24-1.40 (m, 2H), 1.46 (s, 9H), 1.62 (m, 1H), 1.88 (m, 1H), 2.02 (m, 1H), 3.38 (m, 1H), 3.45 (d, 2H, J=7.0 Hz), 3.90 (m, 1H), 4.16 (m, 2H), 5.10-5.20 (m, 2H), 5.94 (m, 1H), 7.14 (m, 1H), 7.96 (d, 1H, J=3.0 Hz); MS (CI/NH3) m/e 352 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06127386 |
| Source dataset | uspto-grants-2000_10 |
| ORD ID | ord-965fb7395b454253900a558106a28998 |
| Source note | uspto-grants-2000_10 |