HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 66803490, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Lithium hydroxide, monohydrate | HCID 168937 | — |
| Reactant | HCID 66802732 | HCID 66802732 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 66803490 | HCID 66803490 | 72.4% |
Reaction Steps
5-(2,2,2-Trifluoroethylamino)-pyridine-2-carboxylic acid methyl ester (Intermediate 280, 75 mg, 0.320 mmol) was dissolved in a mixture of THF (0.75 mL) and water (0.25 mL) and lithium hydroxide monohydrate (27 mg, 0.640 mmol) was added. The mixture was stirred at room temperature for 18 h. The mixture was diluted with water (5 mL), brought to approximately pH 4 by the addition of 1M HCl, then extracted with DCM (4×9 mL). The combined organic extracts were washed with brine (5 mL), dried over sodium sulfate and evaporated under vacuum to afford the title compound as a white solid (51 mg, 72%). Method B HPLC-MS: MH+ requires m/z=221. Found: m/z=221, Rt=1.30 min (100%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08895733B2 |
| Source dataset | uspto-grants-2014_11 |
| ORD ID | ord-4e1b442caee242688910d21ca7d2e66b |
| Source note | uspto-grants-2014_11 |