HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 118378998, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Iodine | HCID 807 | — |
| Reactant | 5-Methylpyrazolo[1,5-a]pyridine-3-carboxylic acid | HCID 19770951 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 118378998 | HCID 118378998 | 94.5% |
Reaction Steps
To a solution of 5-methylpyrazolo[1,5-a]pyridine-3-carboxylic acid (2.11 g) in THF (40 mL) was added 1M lithiumhexadisilazide THF solution (35.9 mL) at 0° C., the mixture was stirred for 30 min, and iodine (3.65 g) was added thereto. The reaction mixture was stirred overnight at room temperature under nitrogen gas atmosphere, 1N hydrochloric acid was added, and the mixture was extracted with ethyl acetate. The extract was washed with aqueous sodium thiosulfate solution, water and saturated brine, and dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was washed with hexane/IPE to give the title compound (3.42 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09296746B2 |
| Source dataset | uspto-grants-2016_03 |
| ORD ID | ord-bd828f6535c14c91a9506dd3c4502814 |
| Source note | uspto-grants-2016_03 |