HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 66972133, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 66973322 | HCID 66973322 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 66972133 | HCID 66972133 | 86.1% |
Reaction Steps
To an 8 mL screw-cap vial was added dioxane (9 mL), 1 N aqueous hydrochloric acid (HCl; 1 mL), and N′-[1-(4-chloro-benzenesulfonyl)-5-fluoro-2-oxo-1,2-dihydro-pyrimidin-4-yl]-N,N-dimethylformamidine (269 mg, 0.75 mmol). The mixture was shaken at room temperature for 16 h, evaporated under a stream of nitrogen, and partitioned between EtOAc and satd aq NaHCO3. The organic phase was dried over MgSO4, filtered, and evaporated to yield the title product as a white solid (196 mg, 86%): mp 174-178° C.; 1H NMR (300 MHz, CDCl3) δ 8.5 (br s, 1H), 8.08 (d, J=5.9 Hz, 1H), 8.04-7.98 (m, 2H), 7.55-7.49 (m, 2H), 5.9 (br s, 1H); ESIMS m/z 304 ([M+H]+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09006259B2 |
| Source dataset | uspto-grants-2015_04 |
| ORD ID | ord-bb424146db7b43c5913d4b5fe40f59ba |
| Source note | uspto-grants-2015_04 |