HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → 2,4-Dichloro-5-((trimethylsilyl)ethynyl)pyrimidine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | Trimethylsilylacetylene | HCID 66111 | — |
| Reactant | 2,4-Dichloro-5-iodopyrimidine | HCID 263438 | — |
| Catalyst | Palladium Chloride | HCID 24290 | — |
| Catalyst | Copper iodide | HCID 83717 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 2,4-Dichloro-5-((trimethylsilyl)ethynyl)pyrimidine | HCID 21080989 | — |
Reaction Steps
66.55 g of 2,4-dichloro-5-iodo-pyrimidine is stirred for three hous in 1.2 litres of absolute THF with 70 ml of triethylamine, 4.9 g of palladium chloride, 13.3 g of triphenylphosphine, 4 g of copper iodide and 39.3 ml of trimethylsilylacetylene at 40° C. After the reaction has ended the solvent is eliminated in vacuo and the dark red oil remaining is subjected to fractional distillation. The product is distilled over at 0.01 Torr and 100° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07709480B2 |
| Source dataset | uspto-grants-2010_05 |
| ORD ID | ord-b5dd52f993c8408d962e101e102d234f |
| Source note | uspto-grants-2010_05 |