化工社化工社 化学情報印刷レポート · 研究参考用
Triethylamine → {3-[3-(2-Fluoro-ethyl)-cyclobutyl]-phenylethynyl}-triisopropyl-silane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | (Triisopropylsilyl)acetylene | HCID 2734682 | — |
| 反応物 | 1-Bromo-3-[3-(2-fluoro-ethyl)-cyclobutyl]-benzene | HCID 59305366 | — |
| 触媒 | Copper iodide | HCID 83717 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 生成物 | {3-[3-(2-Fluoro-ethyl)-cyclobutyl]-phenylethynyl}-triisopropyl-silane | HCID 59305330 | 80.4% |
反応手順
In a CEM snap top microwave vial were combined 1-Bromo-3-[3-(2-fluoro-ethyl)-cyclobutyl]-benzene (0.250 gm 9.72 mmol), triisopropylsilylacetylene (0.22 gm, 1.21 mmol), copper iodide (7 mg, 0.178 mmol), tetrakis(triphenylphosphine)palladium (22 mg, 0.088 mmol) and triethylamine (0.600 g, 5.93 mmol). The vial was quickly agitated then irradiated in a CEM Explorer™ microwave instrument for 30 minutes at 80° C. Purification by column chromatography (hexanes) afforded an oil 349 mg. 1H NMR (400 MHz, DMSO-d6) δ ppm 1.06 (s, 21H) 1.62-1.81 (m, 2H) 1.82-1.97 (m, 1H) 2.00-2.45 (m, 4H) NMR (400 MHz, DMSO-d6) δ ppm 3.31-3.62 (m, 1H) 4.30-4.51 (m, 2H) 7.17-7.41 (m, 4H); MS (EI) m/z 256 [M+·].
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07723368B2 |
| 出典データセット | uspto-grants-2010_05 |
| ORD ID | ord-b3d943fd09aa4dbabfd02a842d180be4 |
| 出典メモ | uspto-grants-2010_05 |