HCID 22327752, compound → HCID 131713231, compound

HRID 279916Notes

Reaction equation

HRID 279916 reaction equation
[Na+].[S:2]([O-:17])([O:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][O:12][S:13]([O-:16])(=[O:15])=[S:14])(=[O:4])=[S:3].[Na+].Cl.[C:20]1([NH:26][C:27]([NH:29][C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=2)=[NH:28])[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1>O>[C:6]1([N+:26]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)=[C:27]([NH2:29])[NH2:28])[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.[C:6]1([N+:29]([C:30]2[CH:31]=[CH:32][CH:33]=[CH:34][CH:35]=2)=[C:27]([NH2:26])[NH2:28])[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.[S:2]([O-:17])([O:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][O:12][S:13]([O-:16])(=[O:15])=[S:14])(=[O:4])=[S:3]

Participants

4

Reactant 2

HCID 22327752HCID 22327752, compoundHCID 178479310HCID 178479310, compound

Product 1

HCID 131713231HCID 131713231, compoundYield 223.5%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent2×

Procedure

A solution of hexamethylene bis(thiosulphate) sodium salt (100 g. 0.282 mol) in 500 ml of water at 70° C. was added slowly to a stirred solution of 133 g (0.568 mol) of diphenylguanidine hydrochloride in 700 ml water. The mixture was cooled and the solid which separated was collected. Recrystallisation from a mixture of equal parts by volume of methanol and toluene gave 154 g (77.1%) of hexamethylene bis(thiosulphate) bis(diphenylguanidinium) salt, m.p. 151°-153° C.

Workup

  1. temperatureThe mixture was cooled
  2. customthe solid which separated
  3. customwas collected
  4. customRecrystallisation
  5. additionfrom a mixture of equal parts by volume of methanol and toluene

Sources & evidence

ORD record
ord-404fe40256bb4969a2f6c7821985df46
Source dataset
uspto-grants-1986_05
Patent number
US04587296

Reaction notes

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