反应 #449936

ord-b02602bf0aa642259b82a73e24d6f1bf

反应方程式

CCN(CCNS(C)(=O)=O)c1ccc(N)c(C)c1.O=S(=O)(O)O
N-ethyl-N-(β-methanesulfonamidoethyl)-3-methyl-4-aminoaniline sulfate
O=C([O-])[O-].[Na+].[Na+]
sodium carbonate
ClC(Cl)Cl
chloroform
O=S(=O)([O-])OOS(=O)(=O)[O-].[NH4+].[NH4+]
ammonium persulfate
CCN(CC)c1ccc(N)c(C)c1
CD-2

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.STIRRINGAfter stirring the reaction solution for one hour
  2. 2
    其他a chloroform layer was separated
  3. 3
    其他the reaction solution was subjected to purification through silica gel column chromatography

实验过程

Into the mixture comprising 0.78 g of Comparative Coupler (C-2), 0.80 g of N-ethyl-N-(β-methanesulfonamidoethyl)-3-methyl-4-aminoaniline sulfate, 3.75 g of sodium carbonate, 60 ml of chloroform and 50 ml of water, a solution of 10 ml of water having dissolved therein 1.65 g of ammonium persulfate was gradually added with stirring at room temperature. After stirring the reaction solution for one hour, a chloroform layer was separated and the reaction solution was subjected to purification through silica gel column chromatography to obtain Azomethine Dye (CD-2). Further, Azomethine Dyes (D-1) to (D-4) were synthesized using the couplers of the present invention in place of Coupler (C-2). ##STR5##

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05871895uspto-grants-1999_02