HRID74266
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
To a solution of 5-(benzoxazol-2-yl)-2-(tetrahydropyran-4-yl)aminoaniline (see Working Example 20-2) (200 mg, 0.646 mmol) in ethanol (5 mL) was added ethyl 3-ethoxy-3-iminopropionate (190 mg, 0.969 mmol), and this was heated to reflux for 2 hours. After the reaction was complete, saturated aqueous sodium hydrogen carbonate solution was added, and this was extracted with ethyl acetate. After the organic layer obtained was dried over anhydrous sodium sulfate, it was filtered and concentrated. The crystals obtained were purified by silica gel column chromatography to yield the title compound (249 mg, 95% yield) as gray crystals.
WORKUP
后处理
- temperaturethis was heated
- temperatureto reflux for 2 hours
- extractionthis was extracted with ethyl acetate
- customAfter the organic layer obtained
- dry with materialwas dried over anhydrous sodium sulfate, it
- filtrationwas filtered
- concentrationconcentrated
- customThe crystals obtained
- customwere purified by silica gel column chromatography