HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 57403866, compound → HCID 57400314, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 57403866 | HCID 57403866 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 57400314 | HCID 57400314 | 66.3% |
Reaction Steps
To a solution of 4-{3-[4-(4-carbamoyl-1-methyl-1H-pyrrol-2-yl)-pyrimidin-2-ylamino]-4-trifluoromethoxy-phenyl}-piperazine-1-carboxylic acid tert-butyl ester (176 mg, 0.314 mmol) in dioxane (3 mL), HCl in dioxane solution (4N, 4 mL) were added. The reaction was stirred at room temperature for 6 hours and the precipitate collected by filtration. The precipitate was dissolved in HCl water solution (0.1N, 30 mL) and washed with dichlorometane (50 mL). The aqueous layers were collected and the title compound precipitated by addition of sodium bicarbonate. The aqueous phase was eliminated by filtration, the solid washed with water (10 mL) and dried under vacuo at 30° C. to yield 96 mg (66%) of the title compound as an hazelnut powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08426417B2 |
| Source dataset | uspto-grants-2013_04 |
| ORD ID | ord-da7a6dc9f47743a599f9c49ad7346b8c |
| Source note | uspto-grants-2013_04 |