HRID1390336

反应详情

EQUATION

反应方程式

HRID 1390336 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Dissolve 2.5 g. of sodium in 500 ml. of liquid ammonia in the presence of a catalytic amount of ferric nitrate. Add dropwise to the resulting suspension over a 20 minute interval a solution containing 24.5 g. of 4-diphenylmethyl pyridine in 600 ml. of ether. Stir the resulting dark red mixture for an additional 20 minutes, then add 13 g. of ethyl bromide dropwise. Add an additional 500 ml. of ammonia, stir overnight, then add 300 ml. of ether followed by 150 ml. of water. Separate the solvent layers. Wash the ether layer with water until neutral, dry and remove the solvent under reduced pressure to a residue. Distill the residue at 192°-200° C./1.6 to 2 mm. and obtain thereby 14.7 g. of the title compound as an orange colored oil.

WORKUP

后处理

  1. dissolutionDissolve 2.5 g
  2. additionAdd dropwise to the resulting suspension over a 20 minute interval a solution
  3. additioncontaining 24.5 g
  4. additionadd 13 g
  5. additionAdd an additional 500 ml
  6. additionadd 300 ml
  7. customSeparate the solvent layers
  8. washWash the ether layer with water until neutral,
  9. customdry
  10. customremove the solvent under reduced pressure to a residue
  11. distillationDistill the residue at 192°-200° C./1.6 to 2 mm
  12. customand obtain