HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 135895256, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | Potassium Hydroxide | HCID 14797 | — |
| Reactant | HCID 136337163 | HCID 136337163 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 135895256 | HCID 135895256 | 12% |
Reaction Steps
1-[7-Chloro-6-(3,4-dimethoxy-benzenesulfonyl)-4-oxo-3,4-dihydro-quinazolin-2-yl]-1H-pyrazole-4-carboxylic acid ethyl ester was combined with THF (5 mL), followed by the addition of a solution of aqueous 1M KOH (2.7 mL, 2.7 mmol), and the mixture was stirred for 16 h. The reaction mixture was cooled in an ice bath, then 1M aqueous HCl (5 mL) and water (5 mL) was added. The resulting precipitate was collected and purified by HPLC to furnish the titled compound (16 mg, 12%). MS (Cl): mass calcd. for C20H15ClN4O7S, 490.0; m/z found, 489.0 [M−H]−. 1H NMR (500 MHz, DMSO-d6): 13.10 (s, 2H), 8.95 (s, 1H), 8.86 (s, 1H), 8.32 (s, 1H), 7.87 (s, 1H), 7.59 (dd, J=8.6, 1.8, 1H), 7.41 (d, J=2.0, 1H), 7.19 (d, J=8.6, 1H), 3.85 (s, 3H), 3.81 (s, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08937078B2 |
| Source dataset | uspto-grants-2015_01 |
| ORD ID | ord-a07bfb9c289449b9a601391010f2727e |
| Source note | uspto-grants-2015_01 |