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HRID 1875152作成日:2026年10月25日
Diisobutylaluminum hydride → 4-chloro-N-({4-chloro-3-[(3-chloro-5-ethylphenyl)oxy]-2-fluorophenyl}methyl)-1-({[2-(trimethylsilyl)ethyl]oxy}methyl)-1H-imidazole-5-carboxamide
https://huagongshe.com/reaction/1875152
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
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| 反応物 | Diisobutylaluminum hydride | HCID 14487 | — |
| 反応物 | N-({3-[(3-bromo-5-chlorophenyl)oxy]-4-chloro-2-fluorophenyl}methyl)-4-chloro-1-({[2-(trimethylsilyl)ethyl]oxy}methyl)-1H-imidazole-5-carboxamide | HCID 68487164 | — |
| 反応物 | HCID 178418750 | HCID 178418750 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 4-chloro-N-({4-chloro-3-[(3-chloro-5-ethylphenyl)oxy]-2-fluorophenyl}methyl)-1-({[2-(trimethylsilyl)ethyl]oxy}methyl)-1H-imidazole-5-carboxamide | HCID 68480876 | — |
反応手順
To a solution of N-({3-[(3-bromo-5-chlorophenyl)oxy]-4-chloro-2-fluorophenyl}methyl)-4-chloro-1-({[2-(trimethylsilyl)ethyl]oxy}methyl)-1H-imidazole-5-carboxamide (112 mg, 0.180 mmol) and 1,1′-bis(diphenylphosphino)ferrocenedichloropalladium(II) dichloromethane complex (7.33 mg, 8.98 μmol) in THF (10 ml) was added DIBAL-H (1.0 M solution in DCM) (2.55 mg, 0.018 mmol), followed by diethylzinc (1.0 M solution in heptane) (22.18 mg, 0.180 mmol). The reaction mixture was stirred for one hour at 60° C., cooled to room temperature, diluted with EtOAc and washed with water. The solvent was removed and the crude material (64 mg) was used directly in the next step without purification. LC-MS (ES+) m/z 572 [M+H].
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08304419B2 |
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| 出典データセット | uspto-grants-2012_11 |
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| ORD ID | ord-b346167d94ca436bb5f5275794eb2d62 |
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| 出典メモ | uspto-grants-2012_11 |
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