HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrogen Peroxide → 2-(2,3-Dihydroxy-propylamino)-4-(6,6-dimethyl-4-oxo-3-trifluoromethyl-4,5,6,7-tetrahydro-indazol-1-yl)-benzamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrogen Peroxide | HCID 784 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 2-(2,3-Dihydroxy-propylamino)-4-(6,6-dimethyl-4-oxo-3-trifluoromethyl-4,5,6,7-tetrahydro-indazol-1-yl)-benzonitrile | HCID 66952936 | — |
| Solvent | Water ethanol | HCID 19096565 | — |
| Product | 2-(2,3-Dihydroxy-propylamino)-4-(6,6-dimethyl-4-oxo-3-trifluoromethyl-4,5,6,7-tetrahydro-indazol-1-yl)-benzamide | HCID 11854691 | 29.5% |
Reaction Steps
2-(2,3-Dihydroxy-propylamino)-4-(6,6-dimethyl-4-oxo-3-trifluoromethyl-4,5,6,7-tetrahydro-indazol-1-yl)-benzonitrile (1.7 g, 4 mmol, 1 eq), NaOH (806 mg, 20 mmol, 5 eq), and H2O2 (3 mL) were dissolved in EtOH-water (4:1) (40 mL). The mixture was microwaved at 120° C. for 15 min, then concentrated to dryness, and purified by flash chromatography, eluted by 10% MeOH in EtOAc to give pure 2-(2,3-Dihydroxy-propylamino)-4-(6,6-dimethyl-4-oxo-3-trifluoromethyl-4,5,6,7-tetrahydroindazol-1-yl)-benzamide (0.52 g, 29% yield). LCMS (m/z): M+H=441.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07358370B2 |
| Source dataset | uspto-grants-2008_04 |
| ORD ID | ord-bc299ca198bb4cfa8d1c5441ecaad257 |
| Source note | uspto-grants-2008_04 |