HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylsulfoxide ethanol → 4-(3-Cyclopropylmethyl-6,6-dimethyl-4-oxo-4,5,6,7-tetrahydro-indazol-1-yl)-benzamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylsulfoxide ethanol | HCID 22338741 | — |
| Reactant | 4-(3-Cyclopropylmethyl-6,6-dimethyl-4-oxo-4,5,6,7-tetrahydro-indazol-1-yl)-benzonitrile | HCID 66952435 | — |
| Solvent | Hydrogen Peroxide | HCID 784 | — |
| Solvent | Sodium Hydroxide | HCID 14798 | — |
| Solvent | Sodium chloride; water | HCID 57417360 | — |
| Product | 4-(3-Cyclopropylmethyl-6,6-dimethyl-4-oxo-4,5,6,7-tetrahydro-indazol-1-yl)-benzamide | HCID 11854688 | 43% |
Reaction Steps
After dissolving the nitrile in 10 mL of 4:1 EtOH-DMSO, approximately 0.1 mL of 1 N NaOH (aq.) and 0.1 mL of 30% H2O2 (aq.) were added and the solution stirred for 1.5 hours. The reaction mixture was poured into brine, extracted with EtOAc (×3), and the combined organics washed with brine (×2). The organic extracts were dried over Na2SO4 and concentrated in vacuo to afford 73.2 mg (43% yield) of 4-(3-Cyclopropylmethyl-6,6-dimethyl-4-oxo-4,5,6,7-tetrahydro-indazol-1-yl)-benzamide as an off-white solid. LCMS (m/z): M+H=339.4.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07906529B2 |
| Source dataset | uspto-grants-2011_03 |
| ORD ID | ord-2f212a023d0e4e9a90e893deb5af5a70 |
| Source note | uspto-grants-2011_03 |