関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | N-(5-sulfamoyl-2,3-dihydro-1H-inden-2-yl)acetamide | HCID 11414131 | — |
| 反応物 | 2-Chloro-5-trifluoromethyl-(1,3,4)thiadiazole | HCID 13246789 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 生成物 | N-[5-(5-Trifluoromethyl-[1,3,4]thiadiazol-2-ylsulfamoyl)-indan-2-yl]-acetamide | HCID 57933510 | — |
反応手順
The mixture of 300 mg of 2-chloro-5-trifluoromethyl-[1,3,4]thiadiazol, 300 mg of N-(5-sulfamoyl-indan-2-yl)-acetamide, 1.8 g cesium carbonate und 10 ml of NMP was stirred at 70° C. for 3 hours. After cooling to room temperature 50 ml of water were added and with 2N hydrochloric acid a pH=3 was adjusted. The product was extracted twice with 30 ml of ethyl acetate, the organic layer was washed with 20 ml of water, dried over sodium sulfate and evaporated in vacuo. The resulting crude material was purified by column chromatography (silica gel, eluent: dichloromethane:methanol=90:10).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07772257B2 |
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| 出典データセット | uspto-grants-2010_08 |
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| ORD ID | ord-a9680995247b467085d5ffb3416ae18a |
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| 出典メモ | uspto-grants-2010_08 |
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