HRID46811

反应详情

EQUATION

反应方程式

HRID 46811 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a mixture of 49.8 g. (0.235 mole) α-phenyl-o-toluic acid, 300 ml. ether and 10 ml. pyridine, add dropwise with stirring 25 ml. (0.35 mole) of thionyl chloride. The resulting mixture is stirred 21 hours at room temperature then filtered and the solvent removed in vacuo. The resulting acid chloride is dissolved in 150 ml. ether and added dropwise to 35.7 g (0.48 mole) of tert.butylamine in 500 ml. of ethyl ether, and the mixture cooled to 0° C. After addition is complete the resulting mixture is stirred 1 hour at room temperature, the layers separated, the ether washed with 100 ml. of water, 100 ml. of 2 N sodium hydroxide and then with water again, dried over magnesium sulfate, filtered and evaporated to give N-tert.butyl-α-phenyl-o-toluamide; m.p. 91°-92° C.

WORKUP

后处理

  1. additionTo a mixture of 49.8 g
  2. stirringThe resulting mixture is stirred 21 hours at room temperature
  3. filtrationthen filtered
  4. customthe solvent removed in vacuo
  5. dissolutionThe resulting acid chloride is dissolved in 150 ml
  6. additionAfter addition
  7. stirringis stirred 1 hour at room temperature
  8. customthe layers separated
  9. washthe ether washed with 100 ml
  10. dry with materialof 2 N sodium hydroxide and then with water again, dried over magnesium sulfate
  11. filtrationfiltered
  12. customevaporated