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HRID 75843作成日:2026年10月25日

Triethylamine → HCID 66572312、化合物

https://huagongshe.com/reaction/75843

反応式

関与物質

役割名称HCID仕込み量
反応物TriethylamineHCID 8471—
反応物Ethyl propiolateHCID 12182—
反応物(1E)-N-hydroxy-4-phenylmethoxybenzenecarboximidoyl chlorideHCID 10901405—
溶媒TolueneHCID 1140—
溶媒Ethyl AcetateHCID 8857—
生成物HCID 66572312HCID 66572312—

反応条件

温度80 °C

反応手順

To (E)-4-(benzyloxy)-N-hydroxybenzimidoyl chloride (7.8 g) in Toluene (78 ml), Ethyl propiolate (7.25 ml) was added and stirred. To this, Et3N (4.58 ml) was added dropwise since reaction was exothermic and the reaction mixture was then heated to 80° C. for 2 hours. The reaction mixture was cooled, diluted with Ethyl acetate and washed successively with 0.1M Aqueous HCl, water and brine. Organic layer was collected and concentrated to obtain dark brown residue which was purified by column chromatography (silica gel, DCM) to obtain pale brown solid which was crystallized from DCM-Petroleum ether to obtain the title compound as off white solid. Yield: 2.83 g (29%); MS (ES+): m/z 324 (M+1); 1HNMR (CDCl3; 300 MHz): δ 7.8 (d, 2H), 7.36-7.47 (m, 5H), 7.28 (s, 1H), 7.1 (d, 2H), 5.14 (s, 2H), 4.48 (q, 2H), 1.45 (t, 3H).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08835428B2
出典データセットuspto-grants-2014_09
ORD IDord-5737acb0d24146cf97b0b0a78c91f7c5
出典メモuspto-grants-2014_09