HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Dimethylformamide → (4-Bromophenylethynyl)trimethylsilane
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Dimethylformamide | HCID 6228 | — |
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | 1-Bromo-2-iodobenzene | HCID 11415 | — |
| Edukt | Trimethylsilylacetylene | HCID 66111 | — |
| Katalysator | Copper iodide | HCID 83717 | — |
| Katalysator | HCID 178418476 | HCID 178418476 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | (4-Bromophenylethynyl)trimethylsilane | HCID 4226980 | 105,9% |
Reaktionsschritte
A mixture of 150 g of 97% bromo iodo benzene, 500 ml of anhydrous dimethylformamide, 100 ml of triethylamine, 50 g of trimethylsilyl acetylene, 2.1 g of copper iodide and 2.22 g of bis-(triphenylphosphine)-palladium (II) dichloride was stirred for 2 hours and then 500 ml of ice-cooled water were added. The mixture was extracted 3 times with 500 ml of ethyl acetate and the organic phase was washed with salt water, then dried over sodium sulfate, and evaporated under reduced pressure to obtain 136.542 g of a brown oil which was purified by distillation under reduced pressure to obtain 106.979 g of the expected product with a boiling point of 75°-82° C. under 0.2 mbar and a melting point of 62° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05707982 |
| Quelldatensatz | uspto-grants-1998_01 |
| ORD ID | ord-020795ec5693400798a1ee4408a40f81 |
| Quellennotiz | uspto-grants-1998_01 |