HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → 5-chloro-4-fluoro-1H-pyrrolo[2,3-b]pyridin-3-amine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Stannous Chloride | HCID 24479 | — |
| Reactant | 5-chloro-4-fluoro-3-nitro-1H-pyrrolo[2,3-b]pyridine | HCID 60205274 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Product | 5-chloro-4-fluoro-1H-pyrrolo[2,3-b]pyridin-3-amine | HCID 58195565 | 77.4% |
Reaction Steps
5-Chloro-4-fluoro-3-nitro-1H-pyrrolo[2,3-b]pyridine (1.20 g, 5.57 mmol) was placed in 6M HCl (30 mL). SnCl2 (5.28 g, 27.8 mmol) was then added, and the reaction was stirred for 30 minutes at room temperature. The reaction was then poured into a mixture of 1M NaOH and ice. The resulting suspension was then raised to a pH of 8 and then extracted with 3:1 DCM:i-PrOH. The combined organic fractions were dried, filtered, and concentrated to give the crude product, which was triturated with 10:1 hexanes:DCM to give the product 5-chloro-4-fluoro-1H-pyrrolo[2,3-b]pyridin-3-amine (0.8 g, 77% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08981085B2 |
| Source dataset | uspto-grants-2015_03 |
| ORD ID | ord-d35158486eff4e71b8b418e0bd0e126c |
| Source note | uspto-grants-2015_03 |