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CAS No. : | 58966-93-1 | MDL No. : | MFCD00074887 |
Formula : | C6H18Cl3N3 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | HNPMVNQYFPWBKI-UHFFFAOYSA-N |
M.W : | 238.59 | Pubchem ID : | 2724990 |
Synonyms : |
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Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302-H315-H319-H335 | Packing Group: | N/A |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
60% | The fourth product (13 g, 22 mmol) was dissolved in concentrated sulfuric acid (30 ml) in a 500 ml round bottom flask and heated to 100 C for 48 hours. First cool in an ice bath at 0 C for 30 minutes.The ice bath was continued and 150 ml of 8 M aqueous HCl was slowly added dropwise (three hours was required).Pour the solution into a 1000ml plastic bottle and place in an ice bath.And slowly poured 450 ml of diethyl ether in batches. In an ice bath, stir with a glass rod for 10 minutes.The magnet was stirred vigorously for 110 minutes. The solid was collected by filtration and the solid was washed with 100 ml of diethyl ether. The vacuum is pumped overnight to obtain the final product of light gray solid (TACN 3HCL)(1.7g, 60%). | |
60% | Lastly the final product of the present invention is prepared by taking a 500 ml round-bottom flask and dissolving 13 g (22 mmol) fourth product in 30 ml concentrated sulfuric acid therein. The solution is heated to 100 C. and reacted for 48 hours. After being cooled in an ice bath at 0 C. for 30 minutes, the solution is maintained in the ice bath and 150 ml 8M hydrochloric acid aqueous solution is slowly dropped into the solution of the fourth product (it takes about 3 hours). The mixed solution is poured into a 1000 ml plastic bottle. Then the plastic bottle is placed in an ice bath and 450 ml ether is slowly dropped into the mixed solution in batches. First use a glass rod to stir the mixture for 10 minutes and then use a magnetic mixer to stir the mixture vigorously for 110 minutes in the ice bath. Filter the mixture to get the solid, wash the solid with 100 ml ether and then vacuum dry the solid overnight to get the final product (TACN.3HCL), light gray solid, 1.7 g (60%). | |
1,4,7-Triazacyclononane Ligand 1,4,7-triazacyclononane was produced according the modified method used by the team of Prof. Wieghardt. In this method the detosylation of the 1,4,7-tris-p-toluenesulfon 1,4,7-triazacylononanamide is performed in 5 minutes in hot sulphuric acid of 180 C. Once the solution has cooled down it is transferred into ether under vigorous stirring. The solution that surfaces is decanted and the residue is dissolved in some boiling water. At boiling temperature drops of concentrated hydrochloric acid are added. The brown crystals that precipitate are drained off and washed with cold hydrochloric acid and then with ethanol and ether. The 1,4,7-triazacyclononane. trihydrochloride thus produced is then processed further as described by Wieghardt et al (K. Wieghardt et al, Chem Ber., 112, 2200 (1979)). _ |