HRID436260

反应详情

EQUATION

反应方程式

HRID 436260 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
30 °C

PROCEDURE

实验过程

There were gradually added to a cooled and stirred solution of 190 grams of 2,6-dichloro-3-nitropyridine and 117 grams of benzyl cyanide in 2 liters of dioxane under a nitrogen atmosphere 64 grams of sodium hydride (80% in white oil). The reaction mixture immediately turned a deep dark blue color, gradually a finely divided precipitate began to separate out, the temperature rose (with cooling with ice water) to 30° C. After 3 hours the mixture was treated with about 20 ml of ethyl alcohol, stirred for another 20 minutes, then filtered with suction. The deep blue sodium salt was dissolved in 1 liter of water, treated with dilute acetic acid until the color changed. The 2-(α-cyanobenzyl)-3-nitro-6-chloropyridine formed crystallized out in pure form. M.P. 165° C; Yield 146 grams.

WORKUP

后处理

  1. additionThere were gradually added to
  2. temperaturea cooled
  3. customto separate out
  4. additionAfter 3 hours the mixture was treated with about 20 ml of ethyl alcohol
  5. filtrationfiltered with suction
  6. dissolutionThe deep blue sodium salt was dissolved in 1 liter of water
  7. additiontreated with dilute acetic acid until the color