HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triacetoxyperiodinane → HCID 68502134, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triacetoxyperiodinane | HCID 159087 | — |
| Reactant | HCID 68499637 | HCID 68499637 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 68502134 | HCID 68502134 | 32.2% |
Reaction Steps
1,1,1-Triacetoxy-1,1-dihydro-1,2-benziodoxol-3(1H)-one (3.52 g, 8.30 mmol) was added to 1-[3-(trifluoromethyl)-7,8-dihydro-[1,2,4]triazolo[4,3-b]pyridazin-6-yl]piperidin-4-ol (2.0 g, 6.91 mmol) in DCM (30 mL). The resulting suspension was stirred at ambient temperature for 90 minutes. The reaction mixture was diluted with DCM (300 mL) and washed with 2M NaOH (2×200 mL). The organic layer was dried over MgSO4, filtered and evaporated to afford crude product. The crude product was purified by flash silica chromatography, elution gradient 5 to 10% MeOH in DCM. Pure fractions were evaporated to dryness to give 1-[3-(trifluoromethyl)-7,8-dihydro-[1,2,4]triazolo[4,3-b]pyridazin-6-yl]piperidin-4-one (0.640 g, 32%) as a solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08258140B2 |
| Source dataset | uspto-grants-2012_09 |
| ORD ID | ord-a022778060d441ce828acdde099b5b26 |
| Source note | uspto-grants-2012_09 |