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Bis(trifluoroacetoxy)iodobenzene → 3-(2,4-Difluoro-phenylsulfanyl)-6-methanesulfonyl-1H-indole-2-carboxylic acid methyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Bis(trifluoroacetoxy)iodobenzene | HCID 102317 | — |
| 反応物 | 2,4-Difluorobenzene-1-thiol | HCID 2737073 | — |
| 反応物 | methyl 6-(methylsulfonyl)-1H-indole-2-carboxylate | HCID 7141904 | — |
| 溶媒 | 1,1,1,3,3,3-Hexafluoro-2-propanol | HCID 13529 | — |
| 生成物 | 3-(2,4-Difluoro-phenylsulfanyl)-6-methanesulfonyl-1H-indole-2-carboxylic acid methyl ester | HCID 11418074 | 88% |
反応手順
A solution of 2-carbomethoxy-6-methylsulfonylindole (750 mg, 2.8 mmol), in 10 mL hexafluoroisopropanol was treated with 2,4-difluorothiophenol (7.5 mmol) followed by addition of PIFA (5.6 mmol). The dark colored solution was stirred overnight then partitioned between methylene chloride and water. After concentration of the methylene chloride layer to 20 mL the product was precipitated by addition of 30 mL hexane. An 88% yield of 3-(2,4-difluoro-phenylsulfanyl)-6-methanesulfonyl-1H-indole-2-carboxylic acid methyl ester was obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06872744B2 |
| 出典データセット | uspto-grants-2005_03 |
| ORD ID | ord-93ee1af161384b4ab582c44460df93e0 |
| 出典メモ | uspto-grants-2005_03 |