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HRID 78284作成日:2026年10月25日

Acetic Acid → 2-((4-(2-Nitroethyl)benzyl)oxy)pyridine

https://huagongshe.com/reaction/78284

反応式

関与物質

役割名称HCID仕込み量
反応物Acetic AcidHCID 176—
反応物WaterHCID 962—
反応物VertellusHCID 22959485—
反応物(E)-2-((4-(2-Nitrovinyl)benzyl)oxy)pyridineHCID 58076258—
溶媒Dimethyl SulfoxideHCID 679—
溶媒Diethyl EtherHCID 3283—
溶媒Ethyl AcetateHCID 8857—
生成物2-((4-(2-Nitroethyl)benzyl)oxy)pyridineHCID 5807626649%

反応手順

To a solution of 2-(4-((E)-2-nitro-vinyl)-benzyloxy)-pyridine described in Manufacturing Example 230-1-3 (30.8 g, 120 mmol) and acetic acid (7.4 mL) in dimethyl sulfoxide (150 mL) was added sodium borohydrate (2.45 g, 64.8 mmol) at 30° C. or below. The reaction solution was stirred for 40 minutes at room temperature. Water, ethyl acetate and diethyl ether were added to the reaction solution at 30° C. or below, which was partitioned into aqueous and organic layers. The aqueous layer was extracted with ethyl acetate. The previously obtained organic layer and the ethyl acetate layer were combined, washed with water (3 times) and aqueous sodium chloride (once), dried over anhydrous magnesium sulfate, and then filtered. The filtrate was concentrated under a reduced pressure. The residue was purified by NH silica gel column chromatography (ethyl acetate:heptane=1:4) to obtain the title compound (15.2 g, 49%).

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-4629484faaaf4b1fa005f795d681f7d8
出典メモuspto-grants-2014_09