HRID1650191

反应详情

EQUATION

反应方程式

HRID 1650191 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 4-(2-naphthoyl)-3,5-dichlorobenzyl bromide (0.633 g, 1.61 mmol) and sodium azide (0.245 g, 3.77 mmol) in 10 ml of ethanol was heated at reflux for 3 hours. The reaction mixture was filtered and the precipitate rinsed with ethanol. The filtrate was concentrated and the residue redissolved in ether. The resulting precipitate was collected and washed thoroughly with ether. Concentration afforded 0.594 g of an oil which slowly crystallized. The crude azide was used in the next step without any further purification.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for 3 hours
  3. filtrationThe reaction mixture was filtered
  4. washthe precipitate rinsed with ethanol
  5. concentrationThe filtrate was concentrated
  6. dissolutionthe residue redissolved in ether
  7. customThe resulting precipitate was collected
  8. washwashed thoroughly with ether
  9. concentrationConcentration