HRID411238
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 6-chloro-4-hydroxy[1,5]naphthyridine-3-carboxylate (Preparation 58, 694 mg), potassium carbonate (588 mg), and iodomethane (264 μL) in DMF (15 mL) is stirred at room temperature for 5 hours. The mixture is poured into water (50 mL), and the solution is extracted with CH2Cl2 (3×50 mL). The organic layers are dried (MgSO4) and concentrated. Trituration with ether (50 mL) affords 473 mg (65%) of the title compound as an off-white solid. Physical Characteristics. 1H NMR (DMSO-d6) δ 8.70, 8.31, 7.90, 4.24, 3.92, 1.29; HRMS (FAB) m/z 267.0535 (C12H11ClN2O3+H). Anal. Found: C, 54.14; H, 4.24; N, 10.58.
WORKUP
后处理
- extractionthe solution is extracted with CH2Cl2 (3×50 mL)
- dry with materialThe organic layers are dried (MgSO4)
- concentrationconcentrated