HRID456364

反应详情

EQUATION

反应方程式

HRID 456364 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In a 200-ml flask equipped with a Soxhlet extractor including molecular sieves 4A as a dehydrating agent, a stirrer, a condenser and a thermometer were placed 21.4 g (100 mmol) of 3,3′-diaminobenzidine, 100 ml of acetone and 3.0 g (50 mmol) of acetic acid, followed by heating under reflux in a nitrogen atmosphere for 3 hours. After cooling to room temperature, acetone was removed under reduced pressure, and the residue was purified by silica gel chromatography to yield 16.5 g (65 mmol) of 3,3′-diaminobenzidine monoisopropanimine [N′-isopropylidene-3,4,3′,4′-biphenyltetramine] and 4.7 g (16 mmol) of 3,3′-diaminobenzidine diisopropanimine [N′,N′″-diisopropylidene-3,4,3′,4′-biphenyltetramine].

WORKUP

后处理

  1. customIn a 200-ml flask equipped with a Soxhlet extractor
  2. temperatureby heating
  3. temperatureunder reflux in a nitrogen atmosphere for 3 hours
  4. customacetone was removed under reduced pressure
  5. customthe residue was purified by silica gel chromatography