HRID725370

反应详情

EQUATION

反应方程式

HRID 725370 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

11.3 g of tin dichloride dihydrate are added to 2.25 g of 3',4'-dimethoxy-5'-nitroacetophenone dissolved in 50 ml of ethanol, whereupon the mixture is stirred at 75° for 30 minutes. Thereupon, the reaction mixture is poured on to 100 g of ice, neutralized with about 300 ml of saturated sodium hydrogen carbonate solution and treated with 150 ml of methylene chloride. The mixture is filtered and the methylene chloride phase is separated. This is dried over sodium sulfate and evaporated, and the residue is recrystallized from ether/petroleum ether. There is obtained 5'-amino-3',4'-dimethoxyacetophenone of m.p. 63°-65°.

WORKUP

后处理

  1. filtrationThe mixture is filtered
  2. customthe methylene chloride phase is separated
  3. dry with materialThis is dried over sodium sulfate
  4. customevaporated
  5. customthe residue is recrystallized from ether/petroleum ether