Potassium bisulfide → 6-Mercaptotetrazolo[4,5-b]pyridazine

HRID 1287633Notes

Reaction equation

HRID 1287633 reaction equation
Cl[C:2]1[CH:3]=[CH:4][C:5]2[N:6]([N:8]=[N:9][N:10]=2)[N:7]=1.[SH-:11].[K+]>C(O)C>[SH:11][C:2]1[CH:3]=[CH:4][C:5]2[N:6]([N:8]=[N:9][N:10]=2)[N:7]=1

Participants

4

Reactant 2

HCID 102109Potassium bisulfideHCID 3022316-Chloro-(1,2,3,4)tetrazolo(1,5-b)pyridazine

Product 1

HCID 1785277156-Mercaptotetrazolo[4,5-b]pyridazine

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

A mixture of 21.3 g. (0.137 mole) of 12 and 20 g. (0.25 mole) of potassium hydrosulfide in 200 ml. of ethanol was refluxed for 2 hours and evaporated to dryness. The residue was dissolved in 100 ml. of water and filtered to remove a small amount of insoluble material. The filtrate was acidified to pH 1 with dil. hydrochloric acid to precipitate (13) as colorless needles which were collected by filtration, washed with 20 ml. of water and dried. Yield 9.80 g. (47%). M.p. 140°-141° C. (dec.).

Workup

  1. additionA mixture of 21.3 g
  2. customevaporated to dryness
  3. dissolutionThe residue was dissolved in 100 ml
  4. filtrationof water and filtered
  5. customto remove a small amount of insoluble material
  6. customto precipitate (13) as colorless needles which
  7. filtrationwere collected by filtration
  8. washwashed with 20 ml
  9. dry with materialof water and dried

Sources & evidence

ORD record
ord-ed7d52a04b4943c7a2a48865ee089373
Source dataset
uspto-grants-1976_10
Patent number
US03985738

Reaction notes

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