Sulfuric Acid → 51264-33-6

HRID 1658340Notes

Reaction equation

HRID 1658340 reaction equation
[Na].[OH:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]([C:21]2[CH:26]=[CH:25][C:24]([O:27][S:28]([OH:31])(=[O:30])=[O:29])=[CH:23][CH:22]=2)([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][N:16]=2)C(OCC)=O)=[CH:5][CH:4]=1.[OH-].[Na+].S(=O)(=O)(O)O.[Na].N1C=CC=CC=1C>>[OH:2][C:3]1[CH:4]=[CH:5][C:6]([CH:9]([C:21]2[CH:26]=[CH:25][C:24]([O:27][S:28]([OH:31])(=[O:30])=[O:29])=[CH:23][CH:22]=2)[C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][N:16]=2)=[CH:7][CH:8]=1

Participants

5

Reactant 4

HCID 1118Sulfuric AcidHCID 14798Sodium HydroxideHCID 86733562HCID 86733562, compoundHCID 86733563HCID 86733563, compound

Product 1

HCID 20858251264-33-6

Procedure

20 g. ethyl α-(4-hydroxyphenyl)-α-(4-sulphoxyphenyl)-2-pyridine-acetate monosodium salt were dissolved in 200 ml. 3% aqueous sodium hydroxide solution and the solution then boiled for 1 hour. After cooling, the pH was adjusted to 7.5 by adding diluted sulphuric acid and then distilled to dryness. The residue was treated with boiling ethanol and insoluble material was filtered off. The ethanol extract was concentrated to a small volume to give, by crystallisation, a high yield of the desired 4-hydroxyphenyl-4-sulphoxyphenyl-(2-pyridyl-methane monosodium salt in the form of colourless crystals which melted at 197° - 199°C. (decomposition).

Workup

  1. temperatureAfter cooling
  2. distillationdistilled to dryness
  3. additionThe residue was treated with boiling ethanol and insoluble material
  4. filtrationwas filtered off
  5. extractionThe ethanol extract
  6. concentrationwas concentrated to a small volume
  7. customto give, by crystallisation

Sources & evidence

ORD record
ord-7a3719908c94423488d8fad8d987d92a
Source dataset
uspto-grants-1976_06
Patent number
US03963732

Reaction notes

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