HRID1599203

反应详情

EQUATION

反应方程式

HRID 1599203 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

3-Amino-4-methoxy benzene sulphonylfluoride (1 part) was stirred in acetic/propionic acid 86/14 vol/vol (15 parts) and cooled to 0°-5° C. Nitrosyl sulphuric acid solution (1.9 parts) was dropwise and stirred at 0°-5° C. for 2 hours. The diazo solution was then added to a stirred mixture of N-ethyl-N-benzyl-m-toluidine (1.3 parts), methanol (50 parts), sulphamic acid (0.5 parts) and sodium acetate (5 parts) stirring in ice/water at 0°-5° C. After stirring for 2 hours under these conditions, the dye was filtered off and washed well with water. The damp solid was slurried in water and re-filtered. The dye was then stirred in methanol at room temperature for 1 hour, filtered, and dried at 50° C. to yield the product, 4-(2-methoxy-5-fluorosulphonylphenylazo)-3-methyl-N-ethyl-N-benzyl aniline (1.5 parts). When applied to polyester materials from an aqueous dispersion, the dye gave yellow shades. λmax 450.

WORKUP

后处理

  1. temperaturecooled to 0°-5° C
  2. stirringAfter stirring for 2 hours under these conditions
  3. filtrationthe dye was filtered off
  4. washwashed well with water
  5. filtrationre-filtered
  6. stirringThe dye was then stirred in methanol at room temperature for 1 hour
  7. filtrationfiltered
  8. customdried at 50° C.