HRID1107995

反应详情

EQUATION

反应方程式

HRID 1107995 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A mixture of 294 g of 2,2-bis(4-nitrophenyl)propane (1.03 mol; prepared as in step c) was charged in an autoclave along with 2 liters of 1,4-dioxane and 25 g of 5% palladium on carbon. The autoclave was purged with nitrogen, then heated at 60° C. for six hours under 500 psi hydrogen pressure. The product mixture was filtered to remove the catalyst, then stripped of solvent by rotary evaporation at reduced pressure. The solid residue was triturated with a small amount of hexane, then collected and dried by suction filtration under a blanket of nitrogen to afford 224.0 g (0.99 mol, 96% of theory) of 4,4'-isopropylidenedianiline (bisaniline-A), m.p. 130-131.5° C.

WORKUP

后处理

  1. customThe autoclave was purged with nitrogen
  2. filtrationThe product mixture was filtered
  3. customto remove the catalyst
  4. customstripped of solvent by rotary evaporation at reduced pressure
  5. customThe solid residue was triturated with a small amount of hexane
  6. customcollected
  7. customdried by suction filtration under a blanket of nitrogen