HRID862058

反应详情

EQUATION

反应方程式

HRID 862058 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 5-bromo-2-methoxymethoxybenzyl chloride (21.6 g), sodium cyanide (8.33 g) and dichloromethane (10 ml) was added, at 15° to 20° C., DMSO (80 ml), followed by stirring for 3 hours at room temperature. The mixture was poured into water, which was subjected to extraction with ethyl acetate. The extract solution was washed with water, dried (anhydrous magnesium sulfate) and concentrated to leave an oily product. The oily product was purified by means of a silica gel column chromatography (eluted with ethyl acetate/hexane) to give 5-bromo-2-methoxymethoxybenzyl cyanide (20.4 g), whose spectrum data are shown below.

WORKUP

后处理

  1. additionwas added, at 15° to 20° C.
  2. extractionwas subjected to extraction with ethyl acetate
  3. washThe extract solution was washed with water
  4. dry with materialdried (anhydrous magnesium sulfate)
  5. concentrationconcentrated
  6. customto leave an oily product
  7. customThe oily product was purified by means of a silica gel column chromatography (eluted with ethyl acetate/hexane)