HRID403492
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
[4-(2-Ethyl-5,7-dimethyl-pyrazolo[1,5-a]pyrimidin-3-ylmethyl)-phenyl]-hydrazine (15) (1.8 g, 6.1 mmol) was dissolved in 40 ml water/AcOH (1:3), and after addition of (E)-ethyl 2-cyano-3-ethoxyacrylate (1.24 g, 7.3 mmol) and sodium acetate (1.1 g, 13.4 mmol) the reaction mixture was stirred for 3 h at 100° C. Sodium carbonate was added (pH 11). The organic layer was extracted 2 times with EtOAc, washed with water and brine, dried over Na2 SO4 and concentrated. The crude product was purified by chromatography (50-90% EtOAc in cyclohexane).
WORKUP
后处理
- extractionThe organic layer was extracted 2 times with EtOAc
- washwashed with water and brine
- customdried over Na2 SO4
- concentrationconcentrated
- customThe crude product was purified by chromatography (50-90% EtOAc in cyclohexane)