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HRID 1178192作成日:2026年10月27日

Triethylamine → Ethyl 2-(E-2-(4-(N,N-dimethylaminomethyl)phenyl)ethen-1-yl)nicotinate

https://huagongshe.com/reaction/1178192

反応式

関与物質

役割名称HCID仕込み量
反応物TriethylamineHCID 8471—
反応物Tri-o-tolylphosphineHCID 80271—
反応物Benzenemethanamine, ar-ethenyl-N,N-dimethyl-HCID 519956—
反応物Ethyl chloronicotinateHCID 2796614—
触媒palladium(II) acetateHCID 167845—
溶媒WaterHCID 962—
溶媒DimethylformamideHCID 6228—
生成物Ethyl 2-(E-2-(4-(N,N-dimethylaminomethyl)phenyl)ethen-1-yl)nicotinateHCID 1181105933.9%

反応条件

温度140 °C

反応手順

6.7 g (39 mmol) of ethyl 2-chloronicotinate, 8.2 g (51 mmol) of 4-(N,N-dimethylaminomethyl)styrene, 9.9 g (98 mmol) of triethylamine, 0.36 g of palladium(II) acetate and 0.96 [lacuna] of tri(o-tolyl)phosphine were mixed in 150 ml of dimethylformamide and, after addition of 1 ml of water, stirred at 140° C. for 13 h. The reaction mixture was then concentrated in vacuo, and the resulting residue was partitioned between ethyl acetate and water. The organic phase was separated off, washed with water, dried and concentrated in vacuo. The residue was then crystallized as oxalate from isopropanol after addition of an equivalent amount of oxalic acid. 4.1 g (27%) of the product were obtained as monooxalate.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07276500B2
出典データセットuspto-grants-2007_10
ORD IDord-7cb28733a5ff47dbacee37355451ca60
出典メモuspto-grants-2007_10