HRID2309138

反应详情

EQUATION

反应方程式

HRID 2309138 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Into a glass vessel equipped with a thermometer, a reflux condenser and a stirrer were fed 1,3-bis(3-aminophenoxy)-5-chlorobenzene (8.2 g, 0.025 mol), 5% Pd-C (made by Japan Engelhardt Co.) (0.25 g), sodium formate (4.3 g, 0.063 mol) and 60% aqueous solution of isopropanol (50 ml), and reaction was carried out under reflux with stirring for 5 hours. After completion of the reaction, the catalyst was removed by filtering while hot, followed by cooling to deposit colorless, prismatic crystals, which were filtered and dried to obtain 1,3-bis(3-aminophenoxy)benzene (6.6 g, yield 90.3%). The purity according to high rate liquid chromatography was 99%. M.P.: 105°~107° C.

WORKUP

后处理

  1. customInto a glass vessel equipped with a thermometer, a reflux condenser and a stirrer
  2. temperatureunder reflux
  3. customAfter completion of the reaction
  4. customthe catalyst was removed
  5. filtrationby filtering while hot,
  6. temperatureby cooling
  7. filtrationprismatic crystals, which were filtered
  8. customdried