化工社化工社 化学情報印刷レポート · 研究参考用
Triethylamine → 2,4-Dichloro-5-((trimethylsilyl)ethynyl)pyrimidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | Trimethylsilylacetylene | HCID 66111 | — |
| 反応物 | 2,4-Dichloro-5-iodopyrimidine | HCID 263438 | — |
| 触媒 | Palladium Chloride | HCID 24290 | — |
| 触媒 | Copper iodide | HCID 83717 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2,4-Dichloro-5-((trimethylsilyl)ethynyl)pyrimidine | HCID 21080989 | — |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07173028B2 |
| 出典データセット | uspto-grants-2007_02 |
| ORD ID | ord-7824264cb5e34335a9bd42873718885b |
| 出典メモ | uspto-grants-2007_02 |