Nitric acid,thallium(3+) salt, trihydrate (9CI) → HCID 19907374, compound

HRID 2371560Notes

Reaction equation

HRID 2371560 reaction equation
[CH2:1]([C:15]1([CH2:21][CH2:22][CH2:23][N:24]([CH3:26])[CH3:25])SCCCS1)[CH2:2][C:3]1([CH2:9][CH2:10][CH2:11][N:12]([CH3:14])[CH3:13])SCCCS1.[OH2:27].[OH2:28].O.[N+]([O-])([O-])=O.[Tl+3].[N+]([O-])([O-])=O.[N+]([O-])([O-])=O>CO.O1CCCC1>[CH3:13][N:12]([CH3:14])[CH2:11][CH2:10][CH2:9][C:3](=[O:28])[CH2:2][CH2:1][C:15](=[O:27])[CH2:21][CH2:22][CH2:23][N:24]([CH3:26])[CH3:25]

Participants

5

Procedure

First, 695 mg of 2,2'-ethylenebis[2-(3-dimethylaminopropyl)-m-dithian] was dissolved in 24 ml of absolute methanol and 6 ml of absolute tetrahydrofuran, and after adding dropwise a solution of 3.12 g of thallium (III) nitrate trihydrate in 18 ml of absolute methanol over 2 minutes while stirring at a room temperature, the mixture was stirred for 30 minutes, filtered to remove insoluble matter, and evaporated under a reduced pressure to remove the solvent. After adding 30 ml of water, the mixture was extracted with 100 ml and 50 ml of chloroform. The extracts were combined, washed with a saturated sodium chloride aqueous solution, dried over magnesium sulfate, filtered, and evaporated under a reduced pressure. The residue was applied to a silica gel column and eluted with chloroform/methanol/triethylamine (80:20:1) to obtain 178 mg of the title compound as a pale yellow liquid.

Workup

  1. stirringthe mixture was stirred for 30 minutes
  2. filtrationfiltered
  3. customto remove insoluble matter
  4. customevaporated under a reduced pressure
  5. customto remove the solvent
  6. additionAfter adding 30 ml of water
  7. extractionthe mixture was extracted with 100 ml and 50 ml of chloroform
  8. washwashed with a saturated sodium chloride aqueous solution
  9. dry with materialdried over magnesium sulfate
  10. filtrationfiltered
  11. customevaporated under a reduced pressure
  12. washeluted with chloroform/methanol/triethylamine (80:20:1)

Sources & evidence

ORD record
ord-9c8d4cc2be6e47528ffd8fe68d776733
Source dataset
uspto-grants-1992_03
Patent number
US05093370

Reaction notes

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