HRID1075319

反应详情

EQUATION

反应方程式

HRID 1075319 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of p-nitrotoluene (0.85 g; 0.05 mol) and para-formaldehyde (1.6 g; 0.05 mol) in concentrated sulfuric acid is added acetamide (8.85 g; 0.15 mol) in increments. This solution is stirred at room temperature for 18 hours. The reaction mixture is then poured onto ice. A precipitate is obtainined which is removed by filtration. This solid material is then mixed with butyl acetate, heated, and filtered while hot to remove insolubles. After cooling, 7.8 g (i.e., 75% yield) of product crystallizes out of solution. The product has the following characteristics: melting point of 141° to 143° C.; i.r. 3275, 1640 and 1660 cm-1 (sh); mass. spec. m/e 208.

WORKUP

后处理

  1. additionThe reaction mixture is then poured onto ice
  2. customis removed by filtration
  3. additionThis solid material is then mixed with butyl acetate
  4. temperatureheated
  5. filtrationfiltered while hot
  6. customto remove insolubles
  7. temperatureAfter cooling
  8. custom7.8 g (i.e., 75% yield) of product crystallizes out of solution