反应 #543544

ord-a4e875c34afd4f75a4db895afccd1b3b

反应方程式

Nc1ccc(-c2ccc(N)c(N)c2)cc1N
3,3′-diaminobenzidine
N=C1CCCCC1.N=C1CCCCC1.N=C1CCCCC1.N=C1CCCCC1.Nc1ccc(-c2ccc(N)c(N)c2)cc1N
3,3′-diaminobenzidine tetracyclohexanimine
收率 90.0%

试剂

反应条件

温度
60°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他In a 200-ml flask equipped with a stirrer, a condenser
  2. 2
    温度by heating
  3. 3
    温度After cooling to room temperature
  4. 4
    其他cyclohexanone was removed under reduced pressure
  5. 5
    其他The residue was purified by silica gel chromatography

实验过程

In a 200-ml flask equipped with a stirrer, a condenser and a thermometer were placed 21.4 g (100 mmol) of 3,3′-diaminobenzidine and 100 ml of cyclohexanone, followed by heating with stirring at 60° C. in a nitrogen atmosphere for 2 hours. After cooling to room temperature, cyclohexanone was removed under reduced pressure. The residue was purified by silica gel chromatography, to yield 48.1 g (90 mmol) of the target 3,3′-diaminobenzidine tetracyclohexanimine [N,N′,N″,N′″-tetracyclohexylidene-3,4,3′,4′-biphenyltetramine] in a yield of 90%.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07186454B2uspto-grants-2007_03