HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 178508022, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | HCID 178526802 | HCID 178526802 | — |
| Solvent | Oxolane--water (1/1) | HCID 21881883 | — |
| Product | HCID 178508022 | HCID 178508022 | 30% |
Reaction Steps
To a solution of 5-nitro-2-(pyridazin-3-yl)pyrimidin-4-ol, 35i-g, (3.0 g, 13.6 mmol) in THF/H2O (100 mL, VTHF/H2O=1:1) was added Na2S204 (4.77 g, 27.4 mmol) and stirred at room temperature for 4 h. The reaction mixture was extracted with EA (100 mL), washed with brine (50 mL), and concentrated under vacuum. The residue was purified by column chromatography to afford the product, 35i-h, (0.8 g, 30%) as a yellow solid. 1H NMR (300 MHz, CD3OD) δ5.66 (s, 2H), 7.39 (s, 1H), 7.80 (dd, J=4.8, 8.4 Hz, 1H), 8.29 (d, J=8.4 Hz, 1H), 9.26 (d, J=4.8 Hz), LC-MS (M+H)+ 190.1.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09079930B2 |
| Source dataset | uspto-grants-2015_07 |
| ORD ID | ord-8530ff0729784f5bb681bd4c315504f8 |
| Source note | uspto-grants-2015_07 |