関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Chloride | HCID 5234 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | N-(pyridin-2-ylmethyl)methanesulfonamide | HCID 4657001 | — |
| 反応物 | 1-(Bromomethyl)-4-(tetradecyloxy)benzene | HCID 10022840 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | N-(2-Pyridinylmethyl)-N-[[4-(tetradecyloxy)phenyl]methyl]methanesulfonamide | HCID 19014986 | 38.3% |
反応手順
To a room temperature slurry of 0.391 g of 50% sodium hydride in 20 ml of dry tetrahydrofuran is added, via cannula, 1.27 g of product from Example 121 in 30 ml of dry tetrahydrofuran. The reaction is stirred at room temperature for 1.5 hours. Two and one half grams of product from Example 20 in 30 ml of dry tetrahydrofuran is added via cannula. The reaction is stirred at room temperature for 20 hours followed by heating at reflux temperature for 2 hours. The cooled reaction is poured into half saturated sodium chloride and extracted with methylene chloride. The combined organic layers are washed with saturated sodium chloride, dried and concentrated in vacuo. The residue is purified by chromatography (silica gel: 40% ethyl acetate/hexane) to give 1.22 g of the desired product as colorless crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05208247 |
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| 出典データセット | uspto-grants-1993_05 |
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| ORD ID | ord-81fb874163f54816a4261f6a54b2ed94 |
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| 出典メモ | uspto-grants-1993_05 |
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