Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 2,4-Dichloro-5-methoxypyrimidine | HCID 601401 | — |
| Reactant | HCID 178418332 | HCID 178418332 | — |
| Reactant | HCID 178461633 | HCID 178461633 | — |
| Catalyst | HCID 22239907 | HCID 22239907 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 86664266 | HCID 86664266 | — |
Reaction Steps
2,4-Dichloro-5-methoxypyrimidine (5 g) was dissolved in THF (50 ml), and while cooling, iron(III) acetylacetone (985 mg) and ethyl magnesium chloride (0.91 M: 36.9 ml) were then added to the solution. The obtained mixture was stirred at room temperature overnight. Thereafter, iron(III) acetylacetone (985 mg) and methyl magnesium chloride (0.91 M: 36.9 ml) were added to the reaction solution further twice. A 1 N hydrochloric acid aqueous solution was added to the reaction mixture, and liquid separation and extraction were then carried out with diethyl ether. The organic layer was dried over magnesium sulfate, and the solvent was then concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (n-heptane:ethyl acetate), so as to obtain the title compound (1 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08268848B2 |
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| Source dataset | uspto-grants-2012_09 |
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| ORD ID | ord-9313fcc820c34415a7e3b7680ca82709 |
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| Source note | uspto-grants-2012_09 |
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