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(1,4-Phenylenebis(methylene))bis(triphenylphosphonium) dibromide → 1,1'-[1,4-Phenylenedi(ethene-2,1-diyl)]bis[4-(pentadecyloxy)benzene]
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | (1,4-Phenylenebis(methylene))bis(triphenylphosphonium) dibromide | HCID 2723797 | — |
| 反応物 | p-Pentadecanoxybenzaldehyde | HCID 23127399 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 1,1'-[1,4-Phenylenedi(ethene-2,1-diyl)]bis[4-(pentadecyloxy)benzene] | HCID 57972946 | 92.9% |
反応手順
In a 30 ml four-necked flask, 7.87 g (23.7 mM) of the p-pentadecanoxybenzaldehyde synthesized above and 8.65 g (11.0 mM) of p-xylylenebis(triphenylphosphonium bromide) were suspended in 100 ml of methanol, and 6.87 g (35.6 mM) of 28 wt % methylate was added dropwise at room temperature (25° C.). The resultant mixture was aged at a refluxing temperature of 65° C. for 3 hours. Methanol was removed by evaporation, and 200 ml of water was added to the residue, and the resultant was stirred. The precipitate formed was collected by filtration, washed with water and acetone, and dried to give 7.49 g of a 1,4-bis(4′-pentadecanoxystyryl)benzene isomeric mixture (compound (1a)). The 1H-NMR data for identification were as follows.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07965534B2 |
| 出典データセット | uspto-grants-2011_06 |
| ORD ID | ord-cdcd12e80e8442a18c2750ed3fe61c68 |
| 出典メモ | uspto-grants-2011_06 |