HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → 10-[1,1-Di(methoxymethyl)-methyl]-1,4,7-tris-(benzyloxycarbonyl)-1,4,7,10-tetraazacyclododecane
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 1,4,7-Tris-(benzyloxycarbonyl)-1,4,7,10-tetrazacyclododecane | HCID 15134258 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | 10-[1,1-Di(methoxymethyl)-methyl]-1,4,7-tris-(benzyloxycarbonyl)-1,4,7,10-tetraazacyclododecane | HCID 18924378 | 400% |
Reaction Steps
39 g (154.6 mmol) of the title compound of Example 5a and 44.43 g (77.3 mmol) of 1,4,7-tris-(benzyloxycarbonyl)-1,4,7,10-tetraazacyclododecane (produced according to Chem. Soc., Perkin Trans. 1, 12:3329, 1991) and 85.14 g (616 mmol) of potassium carbonate in 800 ml acetonitrile are refluxed for 24 hours. Solid is filtered out, and the filtrate is evaporated to dryness in a vacuum. The residue is taken up in 700 ml of methylene chloride and extracted twice with 300 ml of water. The organic phase is dried on magnesium sulfate and concentrated by evaporation in a vacuum. The residue is chromatographed on silica gel (mobile solvent =methylene chloride/methanol 20:1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05747000 |
| Source dataset | uspto-grants-1998_05 |
| ORD ID | ord-eb2cc69e86c84f49867500be9e602217 |
| Source note | uspto-grants-1998_05 |