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HRID 33112作成日:2026年10月24日

Benzamidine → HCID 178510335、化合物

https://huagongshe.com/ja/reaction/33112

反応式

関与物質

役割名称HCID仕込み量
反応物BenzamidineHCID 2332—
反応物2-Propenoic acid, 2-cyano-3-ethoxy-, ethyl esterHCID 78943—
溶媒DimethylformamideHCID 6228—
生成物HCID 178510335HCID 178510335—

反応条件

温度0 °C

反応手順

To a stirred solution of benzamidine (1.0 g, 8.32 mmol) in anhydrous DMF (20 mL ) was added Ethyl(ethoxymethylene)cyanoacetate (11) (1.41 g, 8.32 mmol, 1.0 equiv ) under argon at 0° C. The mixture was stirred at 0° C. for 2 h and increase to 105° C. for 60 h. The reaction mixture was then cooled to ambient temperature. The mixture was extracted with ethyl acetate (2×100 mL ). The combined organic extracts were washed with water (1×50 mL) and brine (1×50 mL), dried (Na2SO4), filtered, and evaporated in vacuo. The residue was washed with water (1×60 mL), dichloromethane (1×60 mL) then dried in the vacuum oven to obtain the light yellow solid as product (0.77 g, 47%). 1H-NMR (CD3CN) δ8.25 (s, 1H ), 8.06 (d, 2H ), 7.70 (t, 1H ), 7.61 (t, 2H). MS LC-MS (MH+=198).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07429584B2
出典データセットuspto-grants-2008_09
ORD IDord-e6425ac839a74fdbb7b9d89eec18c911
出典メモuspto-grants-2008_09