HuagongsheHuagongshe Chemistry Print Report · For research reference only
Allyltributylstannane → 5-Allyl-3-(1-boc-2-(s)-azetidinylmethoxy)pyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Allyltributylstannane | HCID 90628 | — |
| Reactant | (S)-Tert-butyl 2-(((5-bromopyridin-3-YL)oxy)methyl)azetidine-1-carboxylate | HCID 10688713 | — |
| Catalyst | Tetrakis(triphenylphosphine)palladium | HCID 11979704 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | 5-Allyl-3-(1-boc-2-(s)-azetidinylmethoxy)pyridine | HCID 21345179 | 30% |
Reaction Steps
3-(1-BOC-2-(S)-azetidinylmethoxy)-5-bromopyridine (0.95 g, 2.77 mmol) in toluene (10 mL) was added tetrakis(triphenylphosphine) palladium (100 mg) and allyltributyltin (1.72 mL, 5.54 mmol). The mixture was stirred and refluxed for two days. Solvent was evaporated and the residue was chromatographed (silica gel; hexane/EtOAc, 5:1 to 1:1) to afford an oil (250 mg, 30%): 1H NMR (CDCl3, 300 MHz) δ 1.42 (s, 9H), 2.22-2.42 (m, 2H), 3.37 (d, 2H, J=7.0 Hz), 3.87-3.92 (m, 2H), 4.16 (m, 1H), 4.30 (m, 1H), 4.50 (m, 1H), 5.07-5.17 (m, 2H), 5.9 (m, 1H), 7.07 (m, 1H), 8.08 (m, 1H), 8.19 (d, 1H, J=3.0 Hz); MS (CI/NH3) m/z 305 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06127386 |
| Source dataset | uspto-grants-2000_10 |
| ORD ID | ord-3e80b82025a54098871dcba359036998 |
| Source note | uspto-grants-2000_10 |