HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrogen Peroxide → alpha-(2,4-difluorophenyl)-N-[dimethyl(methoxymethyl) methyl]nitrone
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrogen Peroxide | HCID 784 | — |
| Reactant | Sodium Chloride | HCID 5234 | — |
| Reactant | N-(2,4-difluorophenylmethyl)-N-[dimethyl(methoxymethyl)methyl]amine | HCID 21255704 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | alpha-(2,4-difluorophenyl)-N-[dimethyl(methoxymethyl) methyl]nitrone | HCID 72602289 | 51% |
Reaction Steps
A solution of N-(2,4-difluorophenylmethyl)-N-[dimethyl(methoxymethyl)methyl]amine obtained in Example 14 (378.8 mg, 1.65 mmol) and Na2WO4 2H2O (84.3 mg, 0.256 mmol) in methanol (5 ml) was cooled to 0° C. in ice-water bath. To the mixture was added dropwise 31% H2O2 aqueous solution (439.3 mg, 4.00 mmol). After addition the mixture was gradually warmed to room temperature and stirred for 15 hours. The mixture was added to sat. NaCl aqueous solution and extracted three times with ethyl acetate and dried over MgSO4. The mixture was concentrated and purified by silica gel chromatography (toluene/ethyl acetate=5/1) to give the title compound (204.8 mg; 51%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06194461B1 |
| Source dataset | uspto-grants-2001_02 |
| ORD ID | ord-4d225aabeb784a0ca64a287642cac08b |
| Source note | uspto-grants-2001_02 |