HRID1741952

反应详情

EQUATION

反应方程式

HRID 1741952 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

Nine milliliters of diisopropylethylamine were added to 2.11 g of 4,5-(dimethylmethylenedioxy)-3-hydroxy-6-heptenenitrile, and 2 ml of methoxymethyl chloride was then added to the mixture gradually at 0° C. After stir-ring at 0° C. for 16 hours, the reaction mixture was diluted with 300 ml of diethyl ether, and washed with 1N hydrochloric acid, a saturated sodium hydrogen carbonate aqueous solution and a sodium chloride aqueous solution in sequence. The organic layer was dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The obtained residue was filtered by a silica gel column to afford 2.28 g of 4,5-(dimethylmethylenedioxy)-3-methoxymethoxy-6-heptenenitrile having the following properties (yield 88 %).

WORKUP

后处理

  1. additionwas then added to the mixture gradually at 0° C
  2. washwashed with 1N hydrochloric acid
  3. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. filtrationThe obtained residue was filtered by a silica gel column