HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrogen Peroxide → HCID 54591945, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrogen Peroxide | HCID 784 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 54591943 | HCID 54591943 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 54591945 | HCID 54591945 | 77% |
Reaction Steps
To a cooled (0° C.) suspension of 6-(2-(4-fluorophenyl)-2-methylpropylamino)nicotinonitrile (75 mg, 0.28 mmol, 1.0 equiv) and K2CO3 (50 mg, 0.36 mmol, 1.3 equiv) in DMSO (1 mL) was added aq. H2O2 (250 uL, 30% by wt., 2.6 mmol, 9 equiv) by syringe. The reaction was allowed to warm to RT and stirred for 30 minutes. The resulting mixture was diluted with EtOAc and washed three times with satd. aq. LiCl and once with brine. The resulting solution was dried over sodium sulfate, filtered, and concentrated in vacuo. Purification by silica gel chromatography (2%-10% MeOH/DCM) provided the title compound as an off-white foam (54 mg, 77%), (m/z [M+H]=288.1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09133123B2 |
| Source dataset | uspto-grants-2015_09 |
| ORD ID | ord-a9d7fcb30f3b47ba9d83b6e447a73242 |
| Source note | uspto-grants-2015_09 |