HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triacetoxyperiodinane → HCID 86666002, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triacetoxyperiodinane | HCID 159087 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | Sodium Pyrosulfite | HCID 656671 | — |
| Reactant | HCID 67773353 | HCID 67773353 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86666002 | HCID 86666002 | 94.9% |
Reaction Steps
Dess-Martin periodinane (0.25 g, 0.59 mmol) was added to (S)-4-fluoro-N-(1-hydroxy-3-methylbutan-2-yl)-N,3-dimethylbenzamide (Compound Z) (0.1 g, 0.39 mmol) in DCM (3 mL) at rt. The resultant mixture was stirred at rt for 2 h. An aqueous NaHCO3 (8 wt %) solution containing sodium pyrosulphite (0.059 mL, 0.43 mmol) was added and the resultant mixture was stirred vigorously for 15 min. The organic phases was washed with Na2CO3 (8 wt %), filtered through a phase separator and dried using Na2SO4. The solvent was removed under reduced pressure to give the title compound (93 mg, 94%). The obtained crude product was used without further purification. LCMS (M+H)+: 252.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08361998B2 |
| Source dataset | uspto-grants-2013_01 |
| ORD ID | ord-1ad8cd91e0ff42aa8389d20c34606ddf |
| Source note | uspto-grants-2013_01 |