HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanol → HCID 135482279, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 135515411 | HCID 135515411 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 135482279 | HCID 135482279 | 72.3% |
Reaction Steps
A stirred mixture of 2-(2-ethoxy-5-nitrophenyl)-pyrido(3,2-d]pyrimidin-4(3H)-one (Example 19; 1.1 g, 0.00353 mol), stannous chloride dihydrate (4.0 g, 0.0177 mol) and ethanol (15 ml) was heated under reflux for 4 hours. The resulting mixture was allowed to cool, diluted with water (15 ml), adjusted to pH 8 with 2N aqueous sodium hydroxide solution, vigorously shaken with dichloromethane (30 ml), and then this mixture filtered. The aqueous phase was separated and extracted further with dichloromethane (2×30 ml), and the organic extracts were then combined, dried (MgSO4) and evaporated under vacuum. Crystallization of the product from acetonitrile gave the title compound as a hydrated yellow solid (0.72 g, 72%), m.p. 208-210° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06060477 |
| Source dataset | uspto-grants-2000_05 |
| ORD ID | ord-276e66ab14274a96800c16960e8535f1 |
| Source note | uspto-grants-2000_05 |