Nitric acid,thallium(3+) salt, trihydrate (9CI) → HCID 19907374, compound
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
Reactant 2
Product 1
Reagents, catalysts & solvents 2
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
- stirringthe mixture was stirred for 30 minutes
- filtrationfiltered
- customto remove insoluble matter
- customevaporated under a reduced pressure
- customto remove the solvent
- additionAfter adding 30 ml of water
- extractionthe mixture was extracted with 100 ml and 50 ml of chloroform
- washwashed with a saturated sodium chloride aqueous solution
- dry with materialdried over magnesium sulfate
- filtrationfiltered
- customevaporated under a reduced pressure
- 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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