HRID66764

反应详情

EQUATION

反应方程式

HRID 66764 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

A mixture of 41.7 grams (g) of 3-nitrophenol, 24 g of chloroacetonitrile and 58.8 g of anhydrous K2CO3 in 60 milliliters (ml) of DMSO was heated with stirring in a round-bottomed three-necked flask at 70°-80° C. for 3 hours. The reaction mixture was then poured into 1200 ml of ice and water, which resulted in crystal formation. When all of the ice had melted, the solids were filtered, washed well with water and dried overnight in a vacuum oven. The solids were then put in solution in 400 ml of boiling absolute ethanol, treated with activated charcoal and then filtered. The filtrate was cooled to 0° C. and the resulting solids removed by filtration. Drying in a vacuum oven gave 47 g of 3-nitrophenoxyacetonitrile as a pale tan solid having a melting point (m.p.) of 93°-95° C.

WORKUP

后处理

  1. temperaturewas heated
  2. customresulted in crystal formation
  3. filtrationthe solids were filtered
  4. washwashed well with water
  5. customdried overnight in a vacuum oven
  6. additiontreated with activated charcoal
  7. filtrationfiltered
  8. customthe resulting solids removed by filtration
  9. customDrying in a vacuum oven