Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Iodide | HCID 5238 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2-(2-(2-Chloroethoxy)ethoxy)ethanol | HCID 78871 | — |
| Reactant | Tri-tert-butyl 1,4,7,10-Tetraazacyclododecane-1,4,7-triacetate | HCID 11237632 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 19438504 | HCID 19438504 | — |
Reaction Steps
1,4,7,10-Tetraazacyclododecane-4,7,10-triacetic acid tri-t-butyl ester (129 mg, 0.25 mmol) (Example 22(a)) was dissolved in dimethylformamide (1 ml). Sodium iodide (7.5 mg, 0.5 mmol) , triethylamine (76 mg, 0.75 mmol) and 2-[2-(2-chloroethoxy)-ethoxy]ethanol (85 mg, 0.5 mmol) were added to the stirred mixture at ambient temperature. The mixture was stirred at ambient temperature for 90 minutes, the temperature was then raised to 100° C. and kept there for 1 hour. The solvent was evaporated, and the residue was dissolved in dichloromethane (2 ml) and washed with water (1 ml). Trifluoroacetic acid (2 ml) was added to the organic phase and the mixture was stirred at ambient temperature for 1 hour. The solvents were evaporated and the residue dissolved in water (4 ml). The aqueous solution was acidified, the water was evaporated and the title compound was isolated as a hygroscopic white powder. Yield 77 mg (64%). The structure was confirmed by 1HNMR and 13CNMR.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05531978 |
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| Source dataset | uspto-grants-1996_07 |
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| ORD ID | ord-76758d6dffbc4a14a836cd90f48bd9ba |
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| Source note | uspto-grants-1996_07 |
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