Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | 2,4-Dichloro-5-methoxypyrimidine | HCID 601401 | — |
| Reactant | HCID 178418332 | HCID 178418332 | — |
| Catalyst | HCID 22239907 | HCID 22239907 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 71306242 | HCID 71306242 | — |
Reaction Steps
2,4-Dichloro-5-methoxypyrimidine (10 g) was dissolved in THF (100 ml), and while cooling, iron(III) acetylacetone (1.97 g), methyl magnesium chloride (3.0 M: 22.4 ml) were then added to the solution. The obtained mixture was stirred at room temperature overnight. Thereafter, iron(III) acetylacetone (1.97 g), and methyl magnesium chloride (3.0 M: 22.4 ml) were added to the reaction solution further twice. Thereafter, a 1 N hydrochloric acid aqueous solution was added to the reaction mixture, and diethyl ether was then added to the reaction solution to carry out liquid separation and extraction. 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 (6.6 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US08268848B2 |
|---|
| Source dataset | uspto-grants-2012_09 |
|---|
| ORD ID | ord-5108f3e85a6e476ea96bec4af2148b9c |
|---|
| Source note | uspto-grants-2012_09 |
|---|