反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
40 g. of potassium 5-chloro-2-sulfothiophene-3-carboxylate are dissolved in 24 g. of caustic potash dissolved in 400 ml. of water, stirred with 4 g. of activated charcoal, and filtered. 2 g. of palladium/activated charcoal (10% Pd) are then added and the mixture is hydrogenated at room temperature and at an initial pressure of approximately 1 atmosphere until no more hydrogen is taken up. The catalyst is removed by filtration. The filtrate is concentrated by evaporation to 35 ml., and acidified with concentrated HCl to a pH of 1. The precipitate that separates out is redissolved by heating. The resulting solution is cooled to 5°, and the precipitated product is suction filtered without rewashing and dried in vacuo to constant weight, and potassium 2-sulfothiophene-3-carboxylate is obtained.
WORKUP
后处理
- filtrationof activated charcoal, and filtered
- additionof palladium/activated charcoal (10% Pd) are then added
- customis hydrogenated at room temperature
- customThe catalyst is removed by filtration
- concentrationThe filtrate is concentrated by evaporation to 35 ml
- dissolutionThe precipitate that separates out is redissolved
- temperatureby heating
- temperatureThe resulting solution is cooled to 5°
- filtrationfiltered without rewashing
- customdried in vacuo to constant weight