HRID2391838
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
CONDITIONS
反应条件
- 温度
- 150 °C
PROCEDURE
实验过程
A solution of KOH (2.95 g, 52.7 mmol, 10 equiv) in H2O (20 mL) was added to 8-(2-fluoro-3,5-dimethoxy-phenyl)-quinoxaline-5-carbonitrile (Step 94.2) (1.63 g mg, 5.3 mmol) in ethylene glycol (20 mL). The reaction mixture was stirred at 150° C. for 5 h, allowed to cool to rt, diluted with Et2O/H2O, and extracted with Et2O. The aqueous phase was acidified to pH 3 by addition of HCl. The resulting yellow solid was collected by vacuum filtration to provide 1.71 g of the title compound: ESI-MS: 329.1 [M+H]+; tR=4.18 min (System 1).
WORKUP
后处理
- temperatureto cool to rt
- extractionextracted with Et2O
- additionThe aqueous phase was acidified to pH 3 by addition of HCl
- filtrationThe resulting yellow solid was collected by vacuum filtration