HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Chloride → 5-Fluoro-1H-pyrrolo[2,3-b]pyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Chloride | HCID 5234 | — |
| Reactant | Potassium tert-butoxide | HCID 23665647 | — |
| Reactant | 5-Fluoro-3-((trimethylsilyl)ethynyl)pyridin-2-amine | HCID 59706849 | — |
| Solvent | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Product | 5-Fluoro-1H-pyrrolo[2,3-b]pyridine | HCID 20784462 | 94.6% |
Reaction Conditions
| Temperature | 130 °C |
|---|
Reaction Steps
A mixture of 3.80 g of 5-fluoro-3-trimethylsilanylethynylpyrid-2-ylamine and 3.40 g of potassium tert-butoxide in 100 cm3 of 1-methylpyrrolidin-2-one is maintained in the region of 130° C. for about 4 hours. After cooling to a temperature in the region of 20° C., the mixture is poured into 1000 cm3 of saturated aqueous sodium chloride solution and extracted with 5 times 250 cm3 of diethyl oxide. The organic phases are combined, washed with 5 times 100 cm3 of saturated aqueous sodium chloride solution, dried over magnesium sulfate, filtered and concentrated to dryness under reduced pressure (13 kPa). 2.35 g of 5-fluoro-1H-pyrrolo[2,3-b]pyridine are obtained in the form of a solid, the characteristics of which are as follows:
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07968566B2 |
| Source dataset | uspto-grants-2011_06 |
| ORD ID | ord-95464565bfeb40beb0f98b23ad9160cc |
| Source note | uspto-grants-2011_06 |