Potassium Hydroxide → HCID 23715216, compound

HRID 1448581Notes

Reaction equation

HRID 1448581 reaction equation
Cl[C:2]1[S:6][C:5]([S:7]([OH:10])(=[O:9])=[O:8])=[C:4]([C:11]([O-:13])=[O:12])[CH:3]=1.[K+:14].[OH-].[K+]>O>[S:7]([C:5]1[S:6][CH:2]=[CH:3][C:4]=1[C:11]([O-:13])=[O:12])([OH:10])(=[O:8])=[O:9].[K+:14]

Participants

4

Reactant 2

HCID 14797Potassium HydroxideHCID 86736750HCID 86736750, compound

Product 1

HCID 23715216HCID 23715216, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

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

  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

Sources & evidence

ORD record
ord-acf9fcdc4c7b4406af61cf8d624fafe9
Source dataset
uspto-grants-1979_12
Patent number
US04180662

Reaction notes

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