HuagongsheHuagongshe Chemistry Print Report · For research reference only
Formamidine acetate → tert-Butyl 7,8-dihydropyrido[4,3-d]pyrimidine-6(5H)-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Formamidine acetate | HCID 160693 | — |
| Reactant | Sodium ethoxide | HCID 2723922 | — |
| Reactant | tert-butyl 3-[(dimethylamino)methylene]-4-oxotetrahydro-1(2H)-pyridinecarboxylate | HCID 53395404 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | tert-Butyl 7,8-dihydropyrido[4,3-d]pyrimidine-6(5H)-carboxylate | HCID 22707088 | — |
Reaction Steps
Formamidine acetate (472 mg, 4.52 mmol) in 15.0 mL of absolute ethanol was treated with sodium ethoxide (21 wt % solution in ethanol; 1.7 mL). After 30 min, a solution of the product from Step A above (1.15 g) in 8 mL of absolute ethanol was added, and the mixture was warmed at reflux for 18 h. The dark solution was cooled to room temperature and concentrated under reduced pressure, and the residue was partitioned between ethyl acetate and water. The organic layer was separated, washed with brine, dried over magnesium sulfate and concentrated to an orange oil. Purification by flash chromatography (silica gel; 2% methanol/dichloromethane as eluant) afforded the title compound as a light yellow gum.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07388019B2 |
| Source dataset | uspto-grants-2008_06 |
| ORD ID | ord-66ae1acf66014a01b5eaced42a3466dd |
| Source note | uspto-grants-2008_06 |