反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturecooled to 0°-5° C
- stirringAfter stirring for 2 hours under these conditions
- filtrationthe dye was filtered off
- washwashed well with water
- filtrationre-filtered
- stirringThe dye was then stirred in methanol at room temperature for 1 hour
- filtrationfiltered
- customdried at 50° C.