化工社化工社 化学情報印刷レポート · 研究参考用
Trimethylsilylacetylene → 1,4-Dichloro-2-ethynylbenzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Trimethylsilylacetylene | HCID 66111 | — |
| 反応物 | 1,4-Dichloro-2-iodobenzene | HCID 122452 | — |
| 反応物 | Tetrabutylammonium Fluoride | HCID 2724141 | — |
| 触媒 | Copper iodide | HCID 83717 | — |
| 触媒 | Dichlorobis(triphenylphosphine)palladium | HCID 6102075 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1,4-Dichloro-2-ethynylbenzene | HCID 12639754 | 89.3% |
反応手順
The title compound was prepared according to the procedure described in step-5 and step-6 of Intermediate-2 by using 1,4-dichloro-2-iodobenzene (1.0 g, 3.6 mmol), ethynyl(trimethyl)silane (0.541 g, 5.5 mmol), copper iodide (0.027 g, 0.14 mmol), bis(triphenylphosphine) palladium(II) chloride (0.050 g, 0.072 mmol), TBAF (catalytic) and DCM to afford 0.550 g of desired product. 1H NMR (300 MHz, DMSO d6): δ 4.73 (s, 1H), 7.50 (d, J=8.7 Hz, 1H), 7.58 (d, J=8.7 Hz, 1H), 7.71 (s, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09439890B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-190e1ea3be0d4cb89996a786f02a2774 |
| 出典メモ | uspto-grants-2016_09 |