HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 131732358, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 86682241 | HCID 86682241 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 131732358 | HCID 131732358 | 89.3% |
Reaction Steps
To a solution of tert-butyl 1-(5-fluoropyridin-3-yl)-3-methyl-1H-pyrazol-4-yl(prop-2-ynyl)carbamate (1.03 g, 3.11 mmol) in dioxane (5 mL) was added 4 molar (M) hydrogen chloride (HCl; 3.9 mL, 15.5 mmol) in diethyl ether (Et2O). The mixture was stirred at room temperature for 48 h and the resulting white solid was filtered, washed with Et2O and dried under vacuum to give the title compound as a white solid (741 mg, 89%): mp 167-168° C.; 1H NMR (400 MHz, DMSO d6) δ 8.92-8.85 (m, 1H), 8.42 (d, J=2.5 Hz, 1H), 8.15 (s, 1H), 8.12-8.02 (m, 1H), 3.85 (d, J=2.5 Hz, 2H), 3.27-3.19 (m, 1H), 2.22 (s, 3H); ESIMS m/z 230.4 ([M]+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08937083B2 |
| Source dataset | uspto-grants-2015_01 |
| ORD ID | ord-178d8affee5e4e6d93c370415bb9837b |
| Source note | uspto-grants-2015_01 |