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4-Ethynyl-4,4'-dipentylbicyclohexyl → 4-[4-(4-Methoxy-4'-propylbicyclohexyl-4-yl)buta-1,3-diynyl]-4-methoxy-4'-propylbicyclohexyl
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Ethynyl-4,4'-dipentylbicyclohexyl | HCID 15451976 | — |
| 反応物 | 4-Ethynyl-4-methoxy-4'-propylbicyclohexyl | HCID 18364508 | — |
| 反応物 | 4-[4-(4,4'-Dipentylbicyclohexyl-4-yl)buta-1,3-diynyl]-4-methoxy-4'-propylbicyclohexyl | HCID 22013392 | — |
| 触媒 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 触媒 | Cupric acetate monohydrate | HCID 165397 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | 4-[4-(4-Methoxy-4'-propylbicyclohexyl-4-yl)buta-1,3-diynyl]-4-methoxy-4'-propylbicyclohexyl | HCID 22013394 | — |
反応手順
4.00 g of 4-ethynyl-4-methoxy-4′-propylbicyclohexyl, 5.04 g of 4-ethynyl-4,4′-dipentylbicyclohexyl, 10.65 g of copper(II) acetate monohydrate and 0.145 g of copper(I) iodide are refluxed overnight in a mixture of 25 ml of pyridine and 25 ml of methanol. Conventional work-up gives a mixture of the three coupling products 4-[4-(4,4′-dipentylbicyclohexyl-4-yl)buta-1,3-diynyl]-4-methoxy-4′-propylbicyclohexyl (C 76 N 136 I, Δε=0.95, Δn=0.006), 4-[4-(4,4′-dipentylbicyclohexyl-4-yl)buta-1,3-diynyl]-4,4′-dipentylbicyclohexyl and 4-[4-(4-methoxy-4′-propylbicyclohexyl-4-yl)buta-1,3-diynyl]-4-methoxy-4′-propylbicyclohexyl (C 121 N (80) I, Δε=−1.77, Δn=−0.002), which can easily be separated by chromatography.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06203724B1 |
| 出典データセット | uspto-grants-2001_03 |
| ORD ID | ord-ac3ea0183fdc49738a20c64380ee4998 |
| 出典メモ | uspto-grants-2001_03 |