HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hexane → HCID 22404779, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hexane | HCID 8058 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Potassium Persulfate | HCID 24412 | — |
| Reactant | HCID 22404729 | HCID 22404729 | — |
| Catalyst | Copper sulfate pentahydrate | HCID 24463 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 22404779 | HCID 22404779 | 47.5% |
Reaction Steps
By the method of Example 3, Step A, 1.8 grams (0.004 mole) of 3-(5-chloro-3,4-dihydro-2,2-dimethyl-7-fluoro-2H-1-benzopyran-8-yl)-1-methyl-6-trifluoromethyluracil was reacted with 3.5 grams (0.013 mole) of potassium persulfate and 1.1 grams (0.004 mole) of copper(II) sulfate pentahydrate in 30 mL of acetonitrile and 30 mL of water. The crude reaction mixture was subjected to column chromatography on silica gel, with 1:4 ethyl acetate:hexane as the eluant. The product-containing fractions were combined and concentrated under reduced pressure, yielding 0.8 gram of 3-(5-chloro-3,4-dihydro-2,2-dimethyl-7-fluoro-2H-1-benzopyran-4-on-8-yl)-1-methyl-6-trifluoromethyluracil. The NMR spectrum was consistent with the proposed structure.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05521147 |
| Source dataset | uspto-grants-1996_05 |
| ORD ID | ord-cba5941ed1044377a5df9d0be550a1d0 |
| Source note | uspto-grants-1996_05 |