HRID1873580

反应详情

EQUATION

反应方程式

HRID 1873580 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureThe reaction mixture is then warmed to RT
  2. temperatureThe mixture is then heated
  3. temperatureat reflux for 10 h
  4. temperatureAfter cooling
  5. customthe brown precipitate formed
  6. filtrationis filtered off with suction
  7. washwashed three times with a total of 100 ml of ethanol
  8. customdried at 50° C. under reduced pressure
  9. customThe product is used without further purification for the next reaction
  10. customPurification