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
- 0 °C
PROCEDURE
实验过程
870 mg (7.62 mmol) of tetrahydro-2H-pyran-2-carbaldehyde, 504 mg (7.62 mmol) of malononitrile and 626 mg (7.62 mmol) of 3-aminocrotononitrile are dissolved in 8.4 ml of dry ethanol. The solution is cooled to 0° C., and 412 mg (7.62 mmol) of sodium methoxide are added a little at a time. The reaction mixture is then warmed to RT and stirred for 10 min. The mixture is then heated at reflux for 10 h. After cooling, the brown precipitate formed is filtered off with suction, washed three times with a total of 100 ml of ethanol and then dried at 50° C. under reduced pressure. The product is used without further purification for the next reaction. Purification may be carried out by preparative HPLC (column: YMC GEL ODS-AQ S-5, 15 μm; mobile phase gradient: acetonitrile/water 10:90→95:5).
WORKUP
后处理
- temperatureThe reaction mixture is then warmed to RT
- temperatureThe mixture is then heated
- temperatureat reflux for 10 h
- temperatureAfter cooling
- customthe brown precipitate formed
- filtrationis filtered off with suction
- washwashed three times with a total of 100 ml of ethanol
- customdried at 50° C. under reduced pressure
- customThe product is used without further purification for the next reaction
- customPurification