HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrogen Peroxide → HCID 67451802, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrogen Peroxide | HCID 784 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 67452240 | HCID 67452240 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 67451802 | HCID 67451802 | 51% |
Reaction Steps
A 0° C. solution of 2-fluoro-5-(6-(2-(4-fluorophenyl)-2-methylpropylamino)-4-methylpyridazin-3-yl)benzonitrile (0.80 g, 2.2 mmol, 1.0 equiv), 30% hydrogen peroxide (0.45 mL, 4.4 mmol, 2.0 equiv), and K2CO3 (600 mg, 4.4 mmol, 2.0 equiv) in DMSO (9.0 mL) was stirred for 1 hour. The mixture was diluted with EtOAc, washed with saturated NaCl, water and saturated NaCl again, and then dried over Na2SO4. Purification by reverse phase HPLC using a gradient of 20-70% CH3CN/water gave the desired product (420 mg, 51%) as a yellow solid. m/z=379.1 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08969346B2 |
| Source dataset | uspto-grants-2015_03 |
| ORD ID | ord-b572e9ccbc464bbe8ee95a35c23e89cf |
| Source note | uspto-grants-2015_03 |