HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → 5-Chloro-3-(triethyl-silanylethynyl)-pyrazin-2-ylamine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | (Triethylsilyl)acetylene | HCID 637947 | — |
| Reactant | 3-Bromo-5-chloropyrazin-2-amine | HCID 10488609 | — |
| Catalyst | Copper iodide | HCID 83717 | — |
| Catalyst | HCID 178418476 | HCID 178418476 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 5-Chloro-3-(triethyl-silanylethynyl)-pyrazin-2-ylamine | HCID 59463522 | — |
Reaction Steps
A 250 ml round bottom flask was charged with 3-bromo-5-chloro-pyrazin-2-ylamine (2) (1 g, 4.8 mmol), THF (10 ml), copper iodide (9 mg, 0.05 mM) and PdCl2(PPh3)2 (34 mg, 0.05 mmol) under nitrogen. To the reaction mixture, triethylamine (2 ml, 14.4 mmol) and triethylsilylacetylene (1 ml, 5.76 mmol) were added. The reaction mixture was stirred at room temperature for 3 h, then concentrated in vacuo and the residue was purified by flash chromatography, using as eluent pentane/EtOAc 10% to 30%, to give the title compound as an off white solid (1.2 g, 100%). 1H NMR (CDCl3): 0.7-0.8 (6H, qd), 1.0-1.1 (9H, t), 5.0-5.1 (2H, brs), 7.95 (1H, s). MS (ES+): 268.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07795259B2 |
| Source dataset | uspto-grants-2010_09 |
| ORD ID | ord-f28f29cf42754ab08b61aa342508e942 |
| Source note | uspto-grants-2010_09 |