関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrogen Sulfide | HCID 402 | — |
| 反応物 | 3-Fluoropyridine-2-sulfonamide | HCID 19957930 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-Mercaptopyridine-2-sulfonamide | HCID 127427 | — |
反応手順
1.06 g of hydrogen sulfide are passed at a temperature of +16° to +20° C. under a nitrogen atmosphere into a mixture of 6.88 g of potassium tert-butylate and 5 g of 3-fluoropyridin-2-ylsulfonamide in 90 ml of dimethylformamide. After the mixture has been stirred for 41/2 hours at a temperature of +50° C., 0.32 g of potassium tert-butylate are added and 0.1 g of hydrogen sulfide is passed in. After the reaction mixture has been stirred for 2 hours at a temperature of +50° C., it is concentrated in vacuo at a temperature of +75° C. The resulting oily residue is triturated with 135 ml of cold 0.75N sulfuric acid. After the residue has been filtered and washed with a little water, the resulting product is dried in vacuo over phosphorus pentoxide. This gives 3.58 g of 3-mercaptopyridin-2-ylsulfonamide of a melting point of +102° to +104° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05410063 |
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| 出典データセット | uspto-grants-1995_04 |
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| ORD ID | ord-efc3701ebb034da199312f16b9974500 |
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| 出典メモ | uspto-grants-1995_04 |
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