HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 15713224, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Diclofenac | HCID 3033 | — |
| Reactant | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| Reactant | O-Methylhydroxylamine hydrochloride | HCID 521874 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 15713224 | HCID 15713224 | — |
Reaction Steps
A warm solution of 2-[(2,6-dichlorophenyl)amino]-benzeneacetic acid (2.03 g; 7 mmol) in CH2Cl2 (100 mL) is treated with 1,1'-carbonyl-diimidazole (1.75 g; 11 mmol) and the mixture is stirred at room temperature for 5.0 minutes when a clear solution is obtained. The solution is then treated with methoxylamine hydrochloride (1.50 g; 18 mmol) and the reaction mixture stirred at room temperature for 108 hours. It is then decomposed with water, extracted with CH2Cl2, dried over Na2SO4 and then evaporated to dryness to give a solid. Fractional recrystallization of the crude product from a mixture of toluene-CH2Cl2 gives off-white crystalline solid (1.27 g; 55.8%); mp 177°-178° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04943587 |
| Source dataset | uspto-grants-1990_07 |
| ORD ID | ord-da6dc012339447fb9fa911ac81b7ba3e |
| Source note | uspto-grants-1990_07 |