反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 130 °C
PROCEDURE
实验过程
A mixture of 19.4 g of 1,8-dihydroxy-4,5-dinitroanthraquinone, 25.0 g of a mixture consisting of about 72 % of 2-(4-aminophenyl)-ethanol, about 22 % of 2-(4-aminophenyl)propane-1,3-diol, about 3 % of 4-toluidine and by-products, and 140 g of diethylene glycol monomethyl ether is heated to 130° C. over a period of 2.5 hours. Stirring at 130-135° C. is continued for 6 hours, during which the water of the reaction is separated off by distillation. The reaction mixture is cooled to 100° C. and stirred into a mixture of 250 g of water, 250 g of ice and 110 g of 32 % hydrochloric acid. This crude dye suspension is filtered at about 20° C., and the product is washed with about 3 liters of water. After drying, 27 g of a dye mixture containing 65 % of the dye of the formula ##STR12## 13 % of the dye of the formula ##STR13## 3 % of the dye of the formula ##STR14## 7% of 1,8-dihydroxy-4-nitro-5-aminoanthraquinone, and 2-phenylpropane-1,3-diol and phenylethanol is obtained.
WORKUP
后处理
- customthe water of the reaction is separated off by distillation
- temperatureThe reaction mixture is cooled to 100° C.
- stirringstirred into a mixture of 250 g of water, 250 g of ice and 110 g of 32 % hydrochloric acid
- filtrationThis crude dye suspension is filtered at about 20° C.
- washthe product is washed with about 3 liters of water
- customAfter drying
- addition27 g of a dye mixture containing 65 % of the dye of the formula ##STR12## 13 % of the dye of the formula ##STR13## 3 % of the dye of the formula ##STR14## 7% of 1,8-dihydroxy-4-nitro-5-aminoanthraquinone, and 2-phenylpropane-1,3-diol