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HRID 735176作成日:2026年10月26日

Triethylamine → (E)-N-(4'-chlorobiphenyl-4-yl)-3-(4-{[methyl-(4-methylcyclohexyl)amino]methyl}phenyl)acrylamide

https://huagongshe.com/reaction/735176

反応式

関与物質

役割名称HCID仕込み量
反応物TriethylamineHCID 8471—
反応物N,4-DimethylcyclohexanamineHCID 4962029—
反応物4-[(E)-2-(4'-chlorobiphenyl-4-ylcarbamoyl)vinyl]benzyl MethanesulfonateHCID 86601893—
溶媒DichloromethaneHCID 6344—
生成物(E)-N-(4'-chlorobiphenyl-4-yl)-3-(4-{[methyl-(4-methylcyclohexyl)amino]methyl}phenyl)acrylamideHCID 57845832—

反応手順

A reaction mixture of 100 mg (0.226 mmol) of 4-[(E)-2-(4′-chlorobiphenyl-4-ylcarbamoyl)vinyl]benzyl methanesulfonate, 37.34 mg (0.29 mmol) of methyl-(4-methylcyclohexyl)amine, and 0.1 mL of triethylamine in 10 mL of dichloromethane is stirred for 18 hours at ambient temperature. Then the reaction mixture is extracted between water and dichloromethane, the organic phase is separated off, dried, and evaporated down. The residue is purified by column chromatography on silica gel (eluant: dichloromethane/methanol/ammonia (90:10:1)). Yield: 52 mg (49% of theory); C30H33ClN2O (M=473.05); melting point: 227° C.-258° C.; calc.: molecular ion peak (M+H)+: 473/475 (Cl); found: molecular ion peak (M+H)+: 473/475 (Cl); Rf value: 0.48 (silica gel, dichloromethane/methanol/ammonia (90:10:1)).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07592373B2
出典データセットuspto-grants-2009_09
ORD IDord-578f5fe04aba4cb2a44fce535e45c905
出典メモuspto-grants-2009_09