HRID26338

反应详情

EQUATION

反应方程式

HRID 26338 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4.02 g of ammonium chloride and 57 g of zinc powder are added to 180 ml of an aqueous-alcoholic solution (83% of alcohol and 17% of water). This mixture is heated to the reflux temperature, whilst stirring, and 0.122 mol (27 g) of 4-nitro-N-tetrahydrofurfurylaniline is then added gradually. When the reaction medium is decolorised, it is filtered and the filtrate is collected in a flask containing 30 ml of ice-cooled hydrochloric acid (d=1.19). On cooling, the expected dihydrochloride precipitates in the form of crystals. It is filtered off and washed with absolute alcohol and then acetone. After drying in vacuo, it melts at about 190° C. with decomposition.

WORKUP

后处理

  1. temperatureThis mixture is heated to the reflux temperature
  2. filtrationit is filtered
  3. customthe filtrate is collected in a flask
  4. additioncontaining 30 ml of ice-
  5. temperaturecooled hydrochloric acid (d=1.19)
  6. temperatureOn cooling
  7. customthe expected dihydrochloride precipitates in the form of crystals
  8. filtrationIt is filtered off
  9. washwashed with absolute alcohol
  10. customAfter drying in vacuo, it melts at about 190° C. with decomposition