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Dichloromethane → 2-Cyano-1-(4-fluorobenzyl)-5-methanesulfonylindole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Trifluoroacetic acid | HCID 6422 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1-(4-Fluorobenzyl)-5-methanesulfonylindole-2-carboxamide | HCID 22504369 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Cyano-1-(4-fluorobenzyl)-5-methanesulfonylindole | HCID 22504448 | 71.7% |
反応手順
To a mixture of 1-(4-fluorobenzyl)-5-methanesulfonylindole-2-carboxamide (100 mg) and dichloromethane (2 ml), triethylamine (0.09 ml) and anhydrous trifluoroacetic acid (0.09 ml) were added at 15 to 30° C. and the mixture was stirred at the same temperature for 2 hours. Water was added therto, and the mixture was extracted with dichloromethane. The organic layer was washed with water, dried over sodium sulfate and concentrated under reduced pressure. The resulting residue was subjected to silica gel column chromatography (hexane:ethyl acetate=2:1) to obtain 68 mg of the desired product as a white crystal.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06875770B2 |
| 出典データセット | uspto-grants-2005_04 |
| ORD ID | ord-768ae26247fa44bdbc9924daf81bc145 |
| 出典メモ | uspto-grants-2005_04 |