関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Tetraethylene Glycol | HCID 8200 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Methanesulfonate | HCID 85257 | — |
| 反応物 | 1-Phenyl-2,5,8,11-tetraoxatridecan-13-ol | HCID 11076957 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-Phenyl-2,5,8,11,14,17,20,23-octaoxapentacosan-25-ol | HCID 57437703 | 34.5% |
反応手順
To a solution of tetrahydrofuran (140 mL) containing sodium hydride (0.43 g, 18 mmol) was added dropwise a solution of non-polydispersed tetraethylene glycol (3.5 g, 18 mmol) in tetrahydrofuran (10 mL) and the reaction mixture was stirred for 1 h. Then mesylate of non-polydispersed tetraethylene glycol monobenzylether 40 (6.0 g, 16.5 mmol) dissolved in tetrahydrofuran (10 mL) was added dropwise and the reaction mixture was stirred overnight. The crude reaction mixture was filtered through Celite (washed, CH2Cl2, 250 mL) and the filtrate was washed H2O, dried MgSO4, and evaporated to dryness. The resultant oil was chromatographed (silica, ethyl acetate/methanol, 10:1) and chromatographed (silica, chloroform/methanol, 25:1) to afford the non-polydispersed title compound as a clear oil (2.62 g, 34% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07084121B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-746ede52140b4ff6b3a407b25a39a3df |
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| 出典メモ | uspto-grants-2006_08 |
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