HRID1156523

反应详情

EQUATION

反应方程式

HRID 1156523 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
5 °C

PROCEDURE

实验过程

3-(4-(Trifluoromethyl)phenyl)-2,3-dibromopropionitrile (2098 grams) was dissolved in methanol and chilled to 5° C. in an ice-bath. Next, over a 2 hour period, sodium methylate (95%) was added keeping the temperature between 5°-10° C. Following this the reaction mixture was allowed to warm to room temperature, was stirred for 33 hours, and was then stripped to near dryness. Upon the addition of 8 l. ether the mixture was slurried, slowly filtered, and stripped again, resulting in a brown oil. NMR analysis confirmed that the oil was the desired mixture of product.

WORKUP

后处理

  1. custombetween 5°-10° C
  2. temperatureto warm to room temperature
  3. additionUpon the addition of 8 l
  4. filtrationslowly filtered
  5. customresulting in a brown oil
  6. additionmixture of product