HRID1956428
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of ethyl 4-chloro-6-ethoxy-1,5-naphthyridine-3-carboxylate (17.95 g), 4-methoxyaniline (8.29 g), anhydrous potassium carbonate (18.6 g) and THF (250 ml) was stirred at ambient temperature for 48 hours. The mixture was evaporated to dryness and water was added to the residue. The mixture was extracted with dichloromethane to give a solid which was dissolved in IMS (50 ml). The solution was saturated with hydrogen chloride gas whilst cooling the mixture in ice. Ether was added to induce precipitation. The solid was collected by filtration to give ethyl 6-ethoxy-4-(4-methoxyanilino)-1,5-naphthyridine-3-carboxylate hydrochloride, m.p. 160°-162° C. Active (3/3) at 30 mg/kg.
WORKUP
后处理
- customThe mixture was evaporated to dryness and water
- additionwas added to the residue
- extractionThe mixture was extracted with dichloromethane
- customto give a solid which
- temperaturewhilst cooling the mixture in ice
- customprecipitation
- filtrationThe solid was collected by filtration