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HRID 353426作成日:2026年10月26日

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

https://huagongshe.com/reaction/353426

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US06753327B1
出典データセットuspto-grants-2004_06
ORD IDord-474cc3efaa0f4b238426448106145851
出典メモuspto-grants-2004_06