反应 #674283

ord-00d1f0ebe0fa4bef90831e3d948b2145

反应方程式

OO
hydrogen peroxide
CCN(c1ccc(N)cc1)C(C)C.Cl
N-ethyl-N-isopropyl-4-aminoaniline hydrochloride
CCCCOc1ccc(N)cc1N.Cl.Cl
4-butoxybenzene-1,3-diamine dihydrochloride
CCO
ethanol
N
ammonia
CCCCOC1=CC(=Nc2ccc(N(CCO)CCO)cc2)C(N)=CC1=N
2-[[4-(2-amino-5-butoxy-4-iminocyclohexa-2,5-dienylideneamino)phenyl](2-hydroxyethyl)amino]ethanol

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他the ethanol is removed
  2. 2
    其他the coupling product formed
  3. 3
    萃取is extracted with butanol
  4. 4
    其他After removal of the butanol under vacuum

实验过程

To a solution of 0.925 g (0.003 mol) of N-ethyl-N-isopropyl-4-aminoaniline hydrochloride and 0.76 g (0.003 mol) of 4-butoxybenzene-1,3-diamine dihydrochloride in 2 ml of water and 6 ml of ethanol, brought to pH 9.5 with 20% aqueous ammonia, are added 10.2 ml of 6% aqueous hydrogen peroxide solution. After stirring for 24 hours at room temperature, the ethanol is removed and the coupling product formed is extracted with butanol. After removal of the butanol under vacuum, the gummy residue is taken up in ethyl acetate and then in ether. 0.470 g of 2-[[4-(2-amino-5-butoxy-4-iminocyclohexa-2,5-dienylideneamino)phenyl](2-hydroxyethyl)amino]ethanol 10 is obtained in the form of a blue-black powder after drying.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US09226883B2uspto-grants-2016_01