HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 136027595, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Lithium hydroxide, monohydrate | HCID 168937 | — |
| Reactant | HCID 136337177 | HCID 136337177 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 136027595 | HCID 136027595 | 75.8% |
Reaction Steps
Lithium hydroxide monohydrate (28.7 mg, 0.684 mmol) and water (0.29 mL) were added to 1-(4-oxo-3,4,7,8-tetrahydro-[1,4]dioxino[2,3-g]quinazolin-2-yl)-1H-pyrazole-4-carboxylic acid ethyl ester (78.0 mg, 0.228 mmol) in THF (0.85 mL). The reaction mixture was stirred at room temperature for 18 h and was then concentrated and the residue re-dissolved in water (5 mL). This solution was brought to pH 1 with 1M aqueous HCl. The resulting precipitate was collected and dried to yield the titled compound (54.3 mg, 75% yield). MS (ESI/Cl): mass calcd. for C14H10N4O5, 314.1; m/z found, 315.0 [M+H]+. 1H NMR (400 MHz, DMSO-d6): 12.97 (s, 1H), 12.61 (s, 1H), 8.89 (d, J=0.6 Hz, 1H), 8.23 (s, 1H), 7.48 (s, 1H), 7.14 (s, 1H), 4.46-4.29 (m, 4H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08937078B2 |
| Source dataset | uspto-grants-2015_01 |
| ORD ID | ord-786f292f29dc4a7f980ccac0cb7ba2c6 |
| Source note | uspto-grants-2015_01 |