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Sodium Chloride → N-(2-Pyridinylmethyl)-N-(methylsulfonyl)-4-(tetradecyloxy)benzamide
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 | Benzoyl chloride, 4-(tetradecyloxy)- | HCID 9998158 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | N-(2-Pyridinylmethyl)-N-(methylsulfonyl)-4-(tetradecyloxy)benzamide | HCID 19014924 | 90.3% |
反応手順
To a room temperature solution of 0.428 g of washed 50% sodium hydride in 15 ml of dry tetrahydrofuran is added, via cannula, 1.58 g of product from Example 121 dissolved in 20 ml of dry tetrahydrofuran. The mixture is stirred for 2 hours and 3.0 g of product from Example 3 dissolved in 20 ml of dry tetrahydrofuran is added, via cannula. After stirring at room temperature for 30 minutes, the reaction is heated at reflux temperature for 2 hours. The cooled mixture is poured into half saturated sodium chloride and extracted with chloroform. The organic layer is dried and concentrated in vacuo. The residue is purified by chromatography (silica gel: 15-40% ethyl acetate/hexane) to give 3.85 g of the desired product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05208247 |
| 出典データセット | uspto-grants-1993_05 |
| ORD ID | ord-d1044c7f8f5c471bb0204eee3a29fb07 |
| 出典メモ | uspto-grants-1993_05 |