関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Dimethylamine | HCID 674 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 2-Cyano-3-difluoromethoxyphenylsulfonyl chloride | HCID 58100767 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | N,N-Dimethyl-2-cyano-3-difluoromethoxyphenylsulfonamide | HCID 11492812 | — |
反応手順
To a solution of 0.65 g (2.4 mmol) of purified 2-cyano-3-difluoromethoxyphenylsulfonyl chloride in 20 ml of tetrahydrofuran a solution of 274 mg (2.4 mmol) of dimethylamine and 510 mg of sodium carbonate in 15 ml of water was added at room temperature. The reaction mixture was stirred at room temperature for 5 minutes before water was added. The aqueous phase was acidified to pH=1 using hydrochloric acid (10% strength by weight, aqueous solution). The aqueous phase was then extracted three times with dichloromethane. The combined organic extracts were dried over sodium sulfate and filtered. The filtrate was concentrated in vacuo and the resulting residue was triturated with methyl tert-butyl ether. Yield: 0.53 g (79% of theory) of the title compound having a melting point of 100-102° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07563921B2 |
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| 出典データセット | uspto-grants-2009_07 |
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| ORD ID | ord-60568919defe4ae49f601bc989e84393 |
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| 出典メモ | uspto-grants-2009_07 |
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