HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 3-hydroxyiminomethyl-7-methylsulfonylamino-6-phenoxy-4H-1-benzopyran-4-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Reactant | 3-formyl-7-methylsulfonylamino-6-phenoxy-4H-1-benzopyran-4-one | HCID 14722439 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 3-hydroxyiminomethyl-7-methylsulfonylamino-6-phenoxy-4H-1-benzopyran-4-one | HCID 86744200 | 72.3% |
Reaction Steps
4 g of 3-formyl-7-methylsulfonylamino-6-phenoxy-4H-1-benzopyran-4-one was dissolved in 20 ml of N,N-dimethylformamide. Thereto was added 850 mg of hydroxylamine hydrochloride. The mixture was stirred for 1 hour at 20°-25° C. The reaction mixture was mixed with 50 ml of ethyl acetate and 100 ml of water. The organic layer was separated, washed with water and a saturated aqueous sodium chloride solution in this order, and dried with anhydrous magnesium sulfate. The solvent was removed by distillation under reduced pressure. The resulting crystal was recrystallized from ethanol to obtain 3.0 g (yield: 72.3%) of 3-hydroxyiminomethyl-7-methylsulfonylamino-6-phenoxy-4H-1-benzopyran-4-one having a melting point of 199°-200° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04954518 |
| Source dataset | uspto-grants-1990_09 |
| ORD ID | ord-974adaf00a2f476696d992e4d0c46ce5 |
| Source note | uspto-grants-1990_09 |