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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

反応式

関与物質

役割名称HCID仕込み量
反応物Diisobutylaluminum hydrideHCID 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-carboxamideHCID 68487164—
反応物HCID 178418750HCID 178418750—
溶媒TetrahydrofuranHCID 8028—
溶媒Ethyl AcetateHCID 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-carboxamideHCID 68480876—

反応条件

温度60 °C

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

DOI10.6084/m9.figshare.5104873.v1
特許番号US08304419B2
出典データセットuspto-grants-2012_11
ORD IDord-b346167d94ca436bb5f5275794eb2d62
出典メモuspto-grants-2012_11