HRID1448581

反应详情

EQUATION

反应方程式

HRID 1448581 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. filtrationof activated charcoal, and filtered
  2. additionof palladium/activated charcoal (10% Pd) are then added
  3. customis hydrogenated at room temperature
  4. customThe catalyst is removed by filtration
  5. concentrationThe filtrate is concentrated by evaporation to 35 ml
  6. dissolutionThe precipitate that separates out is redissolved
  7. temperatureby heating
  8. temperatureThe resulting solution is cooled to 5°
  9. filtrationfiltered without rewashing
  10. customdried in vacuo to constant weight