関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Cyanomethylenetributylphosphorane | HCID 4622928 | — |
| 反応物 | 4-(methylthio)-1H-indazol-5-ol | HCID 22933648 | — |
| 反応物 | tert-butyl 4-{[4-(methylsulfonyl)-1H-indazol-5-yl]oxy}azepane-1-carboxylate | HCID 22933794 | — |
| 反応物 | HCID 178515017 | HCID 178515017 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | HCID 178503317 | HCID 178503317 | 58% |
反応手順
The 4-(methylthio)-1H-indazol-5-ol (0.166 g, 0.92 mmol) obtained in Example 607 and the trans-2-(4-hydroxycyclohexyl)-1H-isoindole-1,3(2H)-dione (0.151 g, 0.61 mmol) obtained in Example 323, (a) were added to a solution of cyanomethylenetri-n-butylphosphorane (0.247 g, 0.92 mmol) in toluene (6 ml), and the resulting mixture was heated at 100° C. and stirred for 7 hours. The reaction solution was concentrated and then diluted with chloroform, and a 1N-aqueous sodium hydroxide solution was added thereto, followed by extraction with chloroform (three times). The extract solution was dried over anhydrous magnesium sulfate. The solvent was distilled off and the residue was purified by a silica gel chromatography (hexane/ethyl acetate=2/1˜1/1) to obtain 2-(cis-4-{[4-(methylthio)-1H-indazol-5-yl]oxy}cyclohexyl)-1H-isoindole-1,3(2H)-dione (0.144 g: 58%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07199147B2 |
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| 出典データセット | uspto-grants-2007_04 |
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| ORD ID | ord-45618f7a7ec74444834daa30315ddd74 |
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| 出典メモ | uspto-grants-2007_04 |
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