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HRID 720344作成日:2026年10月24日

Ethanol → HCID 21891612、化合物

https://huagongshe.com/ja/reaction/720344

反応式

関与物質

役割名称HCID仕込み量
反応物EthanolHCID 702—
反応物TriethylamineHCID 8471—
反応物3,4,5-Trimethoxy-2-nitrobenzoic acidHCID 97116—
反応物P,P-Diphenylphosphinic azideHCID 199401—
溶媒BenzeneHCID 241—
生成物HCID 21891612HCID 21891612—

反応手順

2-Nitro-3,4,5-trimethoxybenzoic acid (4.7 g) was dissolved in dry benzene (70 mL), triethylamine (2.56 mL) and diphenylphosphoryl azide (4.15 mL) were added to the solution, and the mixture was stirred for 2 hours under reflux. Dry ethanol (140 mL) was added to the reaction mixture, and the mixture was further stirred overnight under reflux. After the reaction mixture was concentrated under reduced pressure, the residue was extracted with ethyl acetate. The resultant organic layer was washed with diluted hydrochloric acid, an aqueous solution of potassium carbonate, water and saturated brine, dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. The residue was purified by column chromatography on silica gel (ethyl acetate:hexane=1:4 to 1:3) to obtain the title compound.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07135473B2
出典データセットuspto-grants-2006_11
ORD IDord-612597d7f3004cada9b8e7790d6814f1
出典メモuspto-grants-2006_11