Ethanol → HCID 135482279, compound

Participants

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 dehydrate (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. Crystallisation of the product from acetonitrile gave the title compound as a hydrated yellow solid (0.72 g, 72%), m.p. 208°-210° C. Found: C,62.88; H,4.88; N,19.67. C15H14N4O2 ;0.25H2O requires C,62.81; H,5.10; N,19.54%.

Provenance & Evidence