Potassium Carbonate → HCID 13138419, compound

HRID 1758298Notes

Reaction equation

HRID 1758298 reaction equation
[CH3:1][N:2]1[C:6]([SH:7])=[N:5][N:4]=[N:3]1.[CH3:8][N:9]1[C:13]([S:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22]Cl)=[N:12][N:11]=[N:10]1.C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[CH3:1][N:2]1[C:6]([S:7][CH2:22][CH2:21][CH2:20][CH2:19][CH2:18][CH2:17][CH2:16][CH2:15][S:14][C:13]2[N:9]([CH3:8])[N:10]=[N:11][N:12]=2)=[N:5][N:4]=[N:3]1

Participants

5

Reactant 3

HCID 11430Potassium CarbonateHCID 20509834HCID 20509834, compoundHCID 178482017HCID 178482017, compound

Product 1

HCID 13138419HCID 13138419, compoundYield 56.5%

Reagents, catalysts & solvents 1

HCID 180AcetoneSolvent

Procedure

1-Methyl-5-mercapto-1,2,3,4-tetrazole (1.2 g) is dissolved in acetone (50 ml). To the solution are added 1-methyl-5-(8-chlorooctyl)thio-1,2,3,4-tetrazole (4.1 g) and potassium carbonate (1.5 g) and the mixture is refluxed for 4 hours. Acetone is distilled off and water is added to the residue. The mixture is extracted with chloroform. The chloroform solution is washed with saturated aqueous sodium chloride and dried over magnesium sulfate. Chloroform is distilled off and the residue is recrystallized from ethyl acetate-hexane to obtain 1-methyl-5-[8-(1-methyl-1,2,3,4-tetrazol-5-yl)thiooctyl]thio-1,2,3,4-tetrazole (2.0 g) as colorless needles, m.p. 52°-54° C.

Workup

  1. temperaturethe mixture is refluxed for 4 hours
  2. distillationAcetone is distilled off
  3. additionwater is added to the residue
  4. extractionThe mixture is extracted with chloroform
  5. washThe chloroform solution is washed with saturated aqueous sodium chloride
  6. dry with materialdried over magnesium sulfate
  7. distillationChloroform is distilled off
  8. customthe residue is recrystallized from ethyl acetate-hexane

Sources & evidence

ORD record
ord-6d02a2d23e4e487bb39cf8bc11462766
Source dataset
uspto-grants-1983_02
Patent number
US04372953

Reaction notes

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