関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Acetonitrile, 2-(methylamino)- | HCID 36652 | — |
| 反応物 | 3-(Trifluoromethyl)phenylmethanesulfonyl chloride | HCID 2794646 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | (N-Methyl-3-Trifluoromethylbenzylsulfonamido)Acetonitrile | HCID 15615993 | — |
反応手順
In this example 21 ml (0.15 mole) of triethylamine was added over a 5 minute period to a cooled solution containing 16 g (0.15 mole) of the hydrochloride salt of methylaminoacetonitrile in 150 ml of methylene chloride. The mixture was stirred at 20° C. for 15 minutes and then 7.9 g (0.1 mole) of pyridine was added. Then 25.9 g (0.1 mole) of 3-trifluoromethylbenzylsulfonylchloride dissolved in about 50 ml methylene chloride was added to the reaction mixture. The reaction mixture was maintained at 20° C. during the addition and then refluxed for three hours. The mixture was cooled to room temperature and washed once with 200 ml of water and then washed twice with 100 ml of aqueous 5 wt. % hydrochloric acid. The washed mixture was dried over magnesium sulfate and evaporated under vacuum affording 28.2 g of the title compound as a solid residue.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04885027 |
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| 出典データセット | uspto-grants-1989_12 |
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| ORD ID | ord-f24e12c018cc49f083d9c820352e343e |
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| 出典メモ | uspto-grants-1989_12 |
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