HRID337064
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
- 100 °C
PROCEDURE
实验过程
3-(3,5-Dibromo-2-oxo-1(2H)-pyrazinyl)-5-fluoro-4-methyl-benzoic acid, ethyl ester (Example 169d, 1.137 g, 2.62 mmol) was dissolved in dioxane (10 mL). α,α-Dimethyl-2-(phenylmethoxy)-benzenemethanamine (Example 134a, 0.63 g) and N-ethyldiisopropylamine (0.67 mL, 3.93 mmol) were added under nitrogen and the resulting solution was stirred at 100° C. for 10 h. The reaction mixture was diluted with water (50 mL), and extracted with ethyl acetate (100 mL×2). The combined organics were dried (MgSO4), filtered and evaporated to afford the crude product. This was purified by (SiO2 chromatography eluting with dichloromethane) to afford the subtitle product (1.55 g).
WORKUP
后处理
- extractionextracted with ethyl acetate (100 mL×2)
- dry with materialThe combined organics were dried (MgSO4)
- filtrationfiltered
- customevaporated
- customto afford the crude product
- customThis was purified by (SiO2 chromatography eluting with dichloromethane)