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HRID 78120作成日:2026年10月26日

Ethanol → HCID 178510832、化合物

https://huagongshe.com/reaction/78120

反応式

関与物質

役割名称HCID仕込み量
反応物EthanolHCID 702—
反応物Potassium CarbonateHCID 11430—
反応物Hydroxylamine HClHCID 21645—
反応物5-Benzyloxy-2-cyanomethylpyridineHCID 22181385—
溶媒WaterHCID 962—
生成物HCID 178510832HCID 17851083227.1%

反応条件

温度70 °C

反応手順

To an ethanol (30 mL) solution of (5-benzyloxy-pyridin-2-yl)-acetonitrile (1.77 g, 7.89 mmol) described in Manufacturing Example 127-1-4 were added hydroxylammonium chloride (848 mg, 11.8 mmol) and potassium carbonate (2.18 g, 15.8 mmol), which was stirred for 11 hours and 20 minutes at 70° C. The mixture was then stirred for another 5 hours and 45 minutes under reflux. Water was added to the reaction mixture at room temperature, which was extracted with ethyl acetate. The organic layer was separated, dried over anhydrous magnesium sulfate, and filtered. The filtrate was concentrated under a reduced pressure, and the residue was purified by silica gel column chromatography (ethyl acetate: methanol=10:1) to obtain the title compound (550 mg, 27%).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08841327B2
出典データセットuspto-grants-2014_09
ORD IDord-1d333c4d82c24031895fb51fc7caa696
出典メモuspto-grants-2014_09