HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,8-Diazabicyclo(5.4.0)undec-7-ene → HCID 88120616, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| Reactant | {4,7,10-Tris[2-(benzyloxy)-2-oxoethyl]-1,4,7,10-tetraazacyclododecan-1-yl}acetic acid | HCID 11193219 | — |
| Reactant | HCID 18764645 | HCID 18764645 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 88120616 | HCID 88120616 | 68% |
Reaction Steps
DBU (820 μL; 5.5 mmol) was added to a suspension of 1,4,7,10-tetraazacyclododecane-1,4,7,10-tetraacetic acid tris(phenylmethyl)ester (prepared according to Step E3 of Example 17) (3.71 g; 5.5 mmol) in toluene (350 mL) obtaining a clear solution, then 2-bromo-N,N-dioctadecylacetamide (prepared according to Example 5, Step A) (3.9 g; 6.05 mmol) dissolved in toluene (50 mL) was added dropwise. After 2 h the reaction mixture was filtered and the solvent was evaporated. The crude was suspended in CH3CN (50 mL) and the insoluble was filtered off with a paper filter. The solution was evaporated obtaining the desired product (4.63 g; 3.74 mmol). Yield 68%. The 13C-NMR, MS and IR spectra were consistent with the structure.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06652834B2 |
| Source dataset | uspto-grants-2003_11 |
| ORD ID | ord-0babd302d29e4562903eebfd0a352948 |
| Source note | uspto-grants-2003_11 |