Hydrogen Sulfide → Potassium bisulfide

HRID 1604900Notes

Reaction equation

HRID 1604900 reaction equation
[OH-].[K+:2].[SH2:3].Cl[C:5]1[N:10]=[N:9][C:8](Cl)=[C:7]2[CH:12]=[N:13][C:14]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)=[CH:15][C:6]=12.[SH-:22].[K+]>C(O)(=O)C.CO>[SH-:3].[K+:2].[SH:3][C:5]1[N:10]=[N:9][C:8]([SH:22])=[C:7]2[CH:12]=[N:13][C:14]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)=[CH:15][C:6]=12

Participants

8

Reactant 4

HCID 402Hydrogen SulfideHCID 14797Potassium HydroxideHCID 102109Potassium bisulfideHCID 12246632HCID 12246632, compound

Product 2

HCID 102109Potassium bisulfideHCID 178527974HCID 178527974, compound

Reagents, catalysts & solvents 2

HCID 176Acetic AcidSolventHCID 887MethanolSolvent

Procedure

Potassium hydrosulfide methanolic solution is prepared by reacting 7 parts by weight of potassium hydroxide, 150 parts by volume of methanol and hydrogen sulfide gas in accordance with the known method. 4.2 parts by weight of 1,4-dichloro-7-phenyl-pyrido[3,4-d]pyridazine is added to the potassium hydrosulfide solution, and the resulting mixture is stirred at room temperature for three hours. Methanol is evaporated under reduced pressure, and the residue is added to 50 parts by volume of water to obtain a solution. The solution is acidified by the addition of acetic acid to precipitate yellow crystals. The crystals are collected by filtration, washed with water and dried to obtain 1,4-dimercapto-7-phenyl-pyrido[3,4-d]pyridazine melting at 212° to 215°C (decomposition).

Workup

  1. customMethanol is evaporated under reduced pressure
  2. additionthe residue is added to 50 parts by volume of water
  3. customto obtain a solution
  4. customto precipitate yellow crystals
  5. filtrationThe crystals are collected by filtration
  6. washwashed with water
  7. customdried

Sources & evidence

ORD record
ord-76f204544c7a49ea8cc04a4794029b44
Source dataset
uspto-grants-1976_04
Patent number
US03948908

Reaction notes

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