HRID128454

反应详情

EQUATION

反应方程式

HRID 128454 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

To a solution of 6.9 g. of phenylhydrazine in 100 ml. of acetic acid is added 10.0 g. of N-(dimethylaminomethylene)isonicotinamide. The reaction mixture is stirred at 90° C. for 1.5 hours and then evaporated in vacuo to an orange oil. This oil is dissolved in 250 ml. of chloroform, washed with 60 ml. of saturated sodium bicarbonate solution, then with 60 ml. of water, dried over sodium sulfate and filtered. The chloroform is removed and the residue is dissolved in 60 ml. of ether. Cooling produces 8.8 g. of the desired product as tan crystals, mp. 92°-94° C.

WORKUP

后处理

  1. customevaporated in vacuo to an orange oil
  2. dissolutionThis oil is dissolved in 250 ml
  3. washof chloroform, washed with 60 ml
  4. dry with materialof water, dried over sodium sulfate
  5. filtrationfiltered
  6. customThe chloroform is removed
  7. dissolutionthe residue is dissolved in 60 ml
  8. temperatureCooling
  9. customproduces 8.8 g