HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,4-Dioxane--water (1/1) → HCID 24753867, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,4-Dioxane--water (1/1) | HCID 21886435 | — |
| Reactant | Potassium hydroxy sulfite | HCID 23707502 | — |
| Reactant | HCID 24753866 | HCID 24753866 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 24753867 | HCID 24753867 | 20% |
Reaction Steps
Oxone (0.43 g, 0.7 mmol) was added in one portion to a stirred solution of 2-isopropyl-4-(5-methyl-1H-pyrazol-3-ylamino)-7-methylsulfanylmethyl-2H-phthalazin-1-one (0.06 g, 0.17 mmol) in a 4:1 mixture of dioxane/water (1.2 ml) and the reaction mixture was stirred at RT for 1 hour. The reaction mixture was diluted with water (5 ml) and the solution was extracted with EtOAc (3×75 ml), the organic layers were combined, dried (MgSO4), filtered and concentrated under vacuum to give the title compound (0.013 g, 20% yield) as a white solid. δH (400 MHz, DMSO) 9.23 (1H, s), 8.48 (1H, d), 8.38 (1H, d), 7.89 (1H, dd), 6.36 (1H, s), 5.33-5.20 (1H, m), 4.77 (2H, s), 2.96 (3H, s), 2.25 (3H, s), 1.33 (6H, d) Tr=1.58 min, m/z (ES+) (M+H)+ 376.24.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07501410B2 |
| Source dataset | uspto-grants-2009_03 |
| ORD ID | ord-d984914711904b51b3b77f5ad24366d3 |
| Source note | uspto-grants-2009_03 |