HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrogen Peroxide → HCID 68873219, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrogen Peroxide | HCID 784 | — |
| Reactant | HCID 57562894 | HCID 57562894 | — |
| Catalyst | HCID 178477782 | HCID 178477782 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 68873219 | HCID 68873219 | — |
Reaction Steps
A mixture of N2-(3-Aminosulfonylphenyl)-5-fluoro-N4-[4-(4-pyridylmethyl)phenyl]-2,4-pyrimidinediamine (50 mg) and methyltrioxorhenium (VII) (5 mg) in THF (15 mL) was treated with 30% aq. H2O2 (23 μL). After 24 h stirring, 30% aq. H2O2 (23 μL) was added and stirred for 24 h. The reaction mixture was filtered through Celite, washed the bed with methanol and concentrated. The residue was purified by HPLC yielded 10 mg of desired product. 1H NMR (DMSO d6, 300 MHz): δ 9.47 (s, 1H), 9.35 (s, 1H), 8.10 (m, 4H), 7.92 (m, 1H), 7.73 (d, 2H, J=8.4 Hz), 7.32-7.18 (m, 8H), 3.91 (s, 2H); LCMS (m/z): 467 (MH+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08399472B2 |
| Source dataset | uspto-grants-2013_03 |
| ORD ID | ord-7266cd54ffef4d31a5c76fefe8f6ed99 |
| Source note | uspto-grants-2013_03 |