関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1,2-Dichloro-1-fluoroethane | HCID 79004 | — |
| 反応物 | 2-Sulfanylbenzene-1-sulfonamide | HCID 11041532 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 2-(2-Chloro-2-fluoroethylthio)-phenylsulfonamide | HCID 19086751 | — |
反応手順
A mixture of 217.8 g of the triethylamine salt of 2-mercaptophenylsulfonamide obtained in accordance with Example P6 and 101 g of 1,2-dichloro-1-fluoroethane in 950 ml of methanol is stirred in an autoclave for 24 hours at a temperature of from +65° C. to +70° C. and for a further 24 hours at from +95° C. to +100° C. The reaction mixture is then concentrated by evaporation and the residue is stirred with water. By extracting with ethyl acetate, washing with water, drying over sodium sulfate, concentrating by evaporation and purifying the residue by chromatography with methylene chloride, 99.5 g (49.2% of the theoretical yield) of 2-(2-chloro-2-fluoroethylthio)-phenylsulfonamide having a melting point of from +88° C. to +89° C. are obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05306693 |
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| 出典データセット | uspto-grants-1994_04 |
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| ORD ID | ord-b03a39ef150a4a4aa23d32bc46f59661 |
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| 出典メモ | uspto-grants-1994_04 |
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