HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Triethylamine → HCID 178418686, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | Triphenylphosphine | HCID 11776 | — |
| Edukt | Trimethylsilylacetylene | HCID 66111 | — |
| Edukt | HCID 178418587 | HCID 178418587 | — |
| Katalysator | Palladium Chloride | HCID 24290 | — |
| Lösungsmittel | Acetonitrile | HCID 6342 | — |
| Produkt | HCID 178418686 | HCID 178418686 | — |
Reaktionsschritte
A mixture of 2.0 g of 3-iodo-4-hydroxy-6-pivaloylaminopyrrolo[2,3-d]pyrimidine, 1.2 g. of trimethylsilylacetylene, 0.1 g of palladium chloride, 0.23 g of triphenylphosphine, 0.06 g of cuprous iodide, and 2.6 g of triethylamine in 100 mL of acetonitrile is heated in a sealed tube for 1.5 hours at 50° C. and then at reflux for 3 hours. The solvent is removed under reduced pressure and the residue triturated with 1:1 ethyl acetate:hexanes and filtered. The solid thus collected is dissolved in methylene chloride and this solution is passed through a pad of silica gel eluting with 1% methanol on methylene chloride. The eluate is concentrated to yield 3-trimethylsilylethynyl-4-hydroxy-6-pivaloylaminopyrrolo[2,3-d]pyrimidine.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05248775 |
| Quelldatensatz | uspto-grants-1993_09 |
| ORD ID | ord-60b4f2f7c4364d6ea701f73a82cf4b0f |
| Quellennotiz | uspto-grants-1993_09 |