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HRID 18256作成日:2026年10月25日

Dichloromethane → (e)-3-[6-[n-(Methoxycarbonylmethyl)amino]pyridin-3-yl]acrylic acid hydrochloride salt

https://huagongshe.com/reaction/18256

反応式

関与物質

役割名称HCID仕込み量
反応物DichloromethaneHCID 6344—
反応物Trifluoroacetic acidHCID 6422—
反応物tert-butyl (E)-3-[6-[N-(methoxycarbonylmethyl)amino]pyridin-3-yl]acrylateHCID 66905699—
生成物(e)-3-[6-[n-(Methoxycarbonylmethyl)amino]pyridin-3-yl]acrylic acid hydrochloride saltHCID 66905135100%

反応手順

A solution of 50% TFA in CH2Cl2 (75 mL) was added to tert-butyl (E)-3-[6-[N-(methoxycarbonylmethyl)amino]pyridin-3-yl]acrylate (5.20 g, 17.8 mmole). The reaction was stirred at room temperature for 45 min then was concentrated under vacuum. The residue was taken up in 4.0 N HCl in dioxane (75 mL), stirred for 5 min, then concentrated to dryness under vacuum. The remaining solid was triturated with 1:1 Et2O/petroleum ether, filtered and dried under vacuum to give the title compound (4.87 g, 100%) as a white solid: MS (ES) m/e 237.2 (M+H)+.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07741339B2
出典データセットuspto-grants-2010_06
ORD IDord-2922442bd0ed47cc8e2481062f9bc4a5
出典メモuspto-grants-2010_06