HRID1389259

反应详情

EQUATION

反应方程式

HRID 1389259 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

In 50 ml of ethanol were dissolved 5.5 g of 3-methylisoxazole-5-carbaldehyde and 3.3 g of nitromethane. To the solution was added dropwise a solution of sodium ethoxide in ethanol, which had been prepared from 1.5 g of sodium and 30 ml of ethanol, while stirring at room temperature. After completion of the dropwise addition, the resultant solution was stirred for a further 3 hrs. at room temperature and then ether was added thereto to separate the sodium salt. This was dissolved in water, which was followed by acidification with hydrochloric acid. The resulting precipitate was filtered off and recrystallized from chloroform to obtain 5.4 g of (3-methylisoxazole-5-yl)glyoxal-2-oxim having m.p. of 179° C.-180° C. Yield, 70%.

WORKUP

后处理

  1. additionAfter completion of the dropwise addition
  2. customto separate the sodium salt
  3. dissolutionThis was dissolved in water
  4. filtrationThe resulting precipitate was filtered off
  5. customrecrystallized from chloroform