HRID23568

反应详情

EQUATION

反应方程式

HRID 23568 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

Zinc powder (10.0 g; 0.15 mol) was added to a stirred mixture of 4-methoxyazobenzene (4.24 g; 20.0 mmol) in 96% ethanol (75 ml) and saturated NH4Cl solution (2.0 ml) at 0° C. (bath temperature). Two more portions of saturated NH4Cl solution (2.0 ml) were added at 1.5 h intervals. The yellowish solution was poured into cold water (100 ml) and filtered. The residue was extracted with methylene chloride (5×50 ml). The combined aqueous phases were extracted with methylene chloride (3×25 ml). The combined organic solutions were,dried (Na2SO4), filtered and evaporated to give 4.3 g crude 1-(4-methoxyphenyl)-2-phenylhydrazine as a reddish oil.

WORKUP

后处理

  1. filtrationfiltered
  2. extractionThe residue was extracted with methylene chloride (5×50 ml)
  3. extractionThe combined aqueous phases were extracted with methylene chloride (3×25 ml)
  4. filtrationfiltered
  5. customevaporated