HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethyl Carbonate → HCID 13259282, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethyl Carbonate | HCID 7766 | — |
| Reactant | Sodium ethoxide | HCID 2723922 | — |
| Reactant | HCID 21452455 | HCID 21452455 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 13259282 | HCID 13259282 | 96.5% |
Reaction Steps
To a mixture of 2.0 g of 2-(m-trifluoromethylanilino)-3-ethylaminomethylpyridine, 1.0 g of sodium ethoxide and 30 ml of dioxane was added dropwise 2.4 g of diethyl carbonate, and the mixture was heated under reflux for 5 hours. After the reaction was complete, the dioxane was removed from the reaction mixture by distillation under reduced pressure. The residue thus obtained was recrystallized from ether to yield 2.1 g of 1-(m-trifluoromethylphenyl)-3-ethyl-2-oxo-1,2,3,4-tetrahydropyrido[2,3-d]pyrimidine as colorless prisms, melting at 155° - 157° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04009166 |
| Source dataset | uspto-grants-1977_02 |
| ORD ID | ord-65a1faf466ac452b9d5f6c5f0e80ddb8 |
| Source note | uspto-grants-1977_02 |