HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hexachloroethane → 5-Chloro-4-fluoro-1-[tris(1-methylethyl)silyl]-1H-pyrrolo[2,3-b]pyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hexachloroethane | HCID 6214 | — |
| Reactant | 4-Fluoro-1-[tris(1-methylethyl)silyl]-1H-pyrrolo[2,3-b]pyridine | HCID 11266334 | — |
| Reactant | CID 53628100 | HCID 178418400 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 5-Chloro-4-fluoro-1-[tris(1-methylethyl)silyl]-1H-pyrrolo[2,3-b]pyridine | HCID 60205273 | 62.6% |
Reaction Steps
4-Fluoro-1-(triisopropylsilyl)-1H-pyrrolo[2,3-b]pyridine (3.0 g, 10.258 mmol) was placed in THF (15 mL) at −78° C. s-BuLi (16.12 mL, 22.57 mmol) was then added dropwise and stirred for 30 minutes. Hexachloroethane (6.07 g, 25.6 mmol) in THF (10 mL) was then added rapidly, and the reaction was stirred for an additional 30 minutes. The reaction was quenched with saturated aqueous NH4Cl and extracted into hexanes. The combined organic fractions were dried, filtered and concentrated to give the crude product that was purified by column chromatography (hexanes) to give 5-chloro-4-fluoro-1-(triisopropylsilyl)-1H-pyrrolo[2,3-b]pyridine (2.1 g, 62% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08981085B2 |
| Source dataset | uspto-grants-2015_03 |
| ORD ID | ord-bc5571b513604a6388393f0a277f4cb3 |
| Source note | uspto-grants-2015_03 |