HuagongsheHuagongshe Chemistry Print Report · For research reference only
Furobufen → 4-Dibenzofuran-2-yl-4-hydroxyiminobutanoic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Furobufen | HCID 38117 | — |
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Reactant | Sodium Acetate Trihydrate | HCID 23665404 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Water | HCID 962 | — |
| Product | 4-Dibenzofuran-2-yl-4-hydroxyiminobutanoic acid | HCID 4226 | 68% |
Reaction Steps
A solution of γ-oxo-2-dibenzofuranbutanoic acid (Example 1) (75.5 g) and sodium acetate trihydrate (114.9 g) in methanol (2.5 L) is treated with a solution of hydroxylamine hydrochloride (38.9 g) in water (150 mL of solution). The solution is heated to reflux for 3.5 hours then concentrated, cooled, and filtered. This solid was washed with water then dried in vacuo to give the crude title compound (71.32 g, 89.6% of theory). This solid was recrystallized from ethyl acetate, washed with hexane, and dried in vacuo to give 53.04 g (68% yield) of the title compound; mp 167-168° C. (d).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05665764 |
| Source dataset | uspto-grants-1997_09 |
| ORD ID | ord-341c309fcc904996acded74ac71bfdd4 |
| Source note | uspto-grants-1997_09 |