HRID1741951

反应详情

EQUATION

反应方程式

HRID 1741951 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
10 °C

PROCEDURE

实验过程

Fifty milliliters of a saturated magnesium sulfate aqueous solution were cooled to 10° C., and 10.23 g of sodium cyanide was gradually added not to proceed over 10° C. After stirring at 10° C. for 45 minutes, a solution of 7.61 g of 1,2-epoxy-3,4-(dimethylmethylenedioxy)-5-hexene in 30 ml of methanol was gradually added to the above mixture not to proceed over 10° C. After stirring at room temperature for 2 hours, the reaction mixture was extracted with ethyl acetate. The extract was washed with a sodium chloride aqueous solution, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography to afford 2.11 g of 4,5-(dimethylmethylenedioxy)-3-hydroxy-6-heptenenitrile having the following properties.

WORKUP

后处理

  1. customto proceed over 10° C
  2. customto proceed over 10° C
  3. stirringAfter stirring at room temperature for 2 hours
  4. extractionthe reaction mixture was extracted with ethyl acetate
  5. washThe extract was washed with a sodium chloride aqueous solution
  6. dry with materialdried over anhydrous magnesium sulfate
  7. concentrationconcentrated under reduced pressure
  8. customThe obtained residue was purified by silica gel column chromatography