HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 5-bromo-4-fluoro-1H-pyrrolo[2,3-b]pyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | 5-Bromo-4-fluoro-1-[tris(1-methylethyl)silyl]-1H-pyrrolo[2,3-b]pyridine | HCID 49758946 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 5-bromo-4-fluoro-1H-pyrrolo[2,3-b]pyridine | HCID 53412938 | 72% |
Reaction Steps
3H2O (80.8 mL, 80.8 mmol; 1.0M solution in THF) was added to 5-bromo-4-fluoro-1-(triisopropylsilyl)-1H-pyrrolo[2,3-b]pyridine (30.0 g, 80.8 mmol) in THF (200 mL) at room temperature. The reaction was stirred for 20 minutes, and then water (200 mL) and ether (500 mL) were added. The aqueous phase was extracted with ether. The combined organic phases were washed with brine, dried (MgSO4) and concentrated in vacuo. The solid was crystallized from EtOAc to provide 5-bromo-4-fluoro-1H-pyrrolo[2,3-b]pyridine (12.5 g, 72% yield). 1H NMR (400 MHz, CDCl3) δ 11.06 (br s, 1H), 8.39 (d, 1H), 7.35 (dd, 1H), 6.60 (dd, 1H); LCMS (APCI+) m/z 214.9, 216.9 (M+H)+, Retention time=2.75 minutes (Method 1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08981085B2 |
| Source dataset | uspto-grants-2015_03 |
| ORD ID | ord-1a58e7b7653d4a9d8ee3b81596d15e25 |
| Source note | uspto-grants-2015_03 |