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HRID 2048373作成日:2026年10月27日
Cyclobutane-1,1-diyldimethanol → 4'-{[4-(6,13-Dioxadispiro[3.2.5.2]tetradec-10-yl)-5-oxo-7-propyl-4,5-dihydro[1,2,4]triazolo[1,5-a]pyrimidin-6-yl]methyl}-3'-fluorobiphenyl-2-carbonitrile
https://huagongshe.com/reaction/2048373
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
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| 反応物 | Cyclobutane-1,1-diyldimethanol | HCID 4498243 | — |
| 反応物 | 3'-Fluoro-4'-{[5-oxo-4-(4-oxocyclohexyl)-7-propyl-4,5-dihydro[1,2,4]triazolo[1,5-a]pyrimidin-6-yl]methyl}biphenyl-2-carbonitrile | HCID 67008884 | — |
| 触媒 | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 4'-{[4-(6,13-Dioxadispiro[3.2.5.2]tetradec-10-yl)-5-oxo-7-propyl-4,5-dihydro[1,2,4]triazolo[1,5-a]pyrimidin-6-yl]methyl}-3'-fluorobiphenyl-2-carbonitrile | HCID 67009616 | 86% |
反応手順
A mixture of 3′-fluoro-4′-{[5-oxo-4-(4-oxocyclohexyl)-7-propyl-4,5-dihydro[1,2,4]triazolo[1,5-a]pyrimidin-6-yl]methyl}biphenyl-2-carbonitrile (3.5 g), cyclobutane-1,1-diyldimethanol (1 g), p-toluenesulfonic acid monohydrate (0.014 g) and toluene (60 mL) was subjected to an azeotropic dehydration reaction by stirring at 110° C. for 16 hr in a reaction vessel equipped with a Dean-stark trap. The reaction mixture was concentrated, and the obtained residue was purified by silica gel column chromatography to give the title compound as a colorless solid (3.6 g, 86%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08592431B2 |
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| 出典データセット | uspto-grants-2013_11 |
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| ORD ID | ord-2e7047ce758e47f1b1bc3fd7db240ace |
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| 出典メモ | uspto-grants-2013_11 |
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