HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phthalic Anhydride → 3-Chloro-4-methoxy-2,5-dimethylpyridine 1-oxide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phthalic Anhydride | HCID 6811 | — |
| Reactant | Sodium Thiosulfate | HCID 24477 | — |
| Reactant | Carbamide Peroxide | HCID 31294 | — |
| Reactant | 3-Chloro-4-methoxy-2,5-dimethylpyridine | HCID 58201214 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 3-Chloro-4-methoxy-2,5-dimethylpyridine 1-oxide | HCID 14369154 | 91.5% |
Reaction Steps
The above 3-chloro-4-methoxy-2,5-dimethylpyridine (181 mg) was dissolved in 5 ml of dichloromethane, and urea peroxide (169 mg) and phthalic anhydride (219 mg) were then added to the solution. The resulting mixture was stirred at room temperature for 2.5 hours. Thereafter, a saturated aqueous sodium thiosulfate solution was added to the reaction solution under cooling on ice, and the resulting mixture was then diluted with chloroform. The water layer was extracted with chloroform two times. The organic layer was dried over anhydrous sodium sulfate, and the solvent was then distilled away, so as to obtain the title compound (181 mg) as a solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08445504B2 |
| Source dataset | uspto-grants-2013_05 |
| ORD ID | ord-1b504b8357834bb68bcbe1d9d5ffcdd3 |
| Source note | uspto-grants-2013_05 |