참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Dimethylamine | HCID 674 | — |
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | 2-Cyano-3-difluoromethoxyphenylsulfonyl chloride | HCID 58100767 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | N,N-Dimethyl-2-cyano-3-difluoromethoxyphenylsulfonamide | HCID 11492812 | — |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07563921B2 |
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| 출처 데이터셋 | uspto-grants-2009_07 |
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| ORD ID | ord-60568919defe4ae49f601bc989e84393 |
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| 출처 메모 | uspto-grants-2009_07 |
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