참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Cyanomethylenetributylphosphorane | HCID 4622928 | — |
| 반응물 | 4-(methylthio)-1H-indazol-5-ol | HCID 22933648 | — |
| 반응물 | tert-butyl 4-{[4-(methylsulfonyl)-1H-indazol-5-yl]oxy}azepane-1-carboxylate | HCID 22933794 | — |
| 반응물 | HCID 178515017 | HCID 178515017 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | HCID 178503317 | HCID 178503317 | 58% |
반응 단계
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%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07199147B2 |
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| 출처 데이터셋 | uspto-grants-2007_04 |
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| ORD ID | ord-45618f7a7ec74444834daa30315ddd74 |
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| 출처 메모 | uspto-grants-2007_04 |
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