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HRID 1918352作成日:2026年10月26日

Phenyl chloroformate → 5-[2-(3-Chloro-phenyl)-ethoxy]-4-ethyl-4H-pyridine-1,3-dicarboxylic acid 3-ethyl ester 1-phenyl ester

https://huagongshe.com/reaction/1918352

反応式

関与物質

役割名称HCID仕込み量
反応物Phenyl chloroformateHCID 15891—
反応物5-[2-(3-Chloro-phenyl)-ethoxy]-nicotinic Acid Ethyl EsterHCID 67169864—
反応物HCID 178418443HCID 178418443—
溶媒TetrahydrofuranHCID 8028—
生成物5-[2-(3-Chloro-phenyl)-ethoxy]-4-ethyl-4H-pyridine-1,3-dicarboxylic acid 3-ethyl ester 1-phenyl esterHCID 67171259—

反応条件

温度-30 °C

反応手順

The compound of step 1 (100 mg, 0.327 mmol) was dissolved in THF (1.5 ml) and the mixture was cooled to −30° C. Phenyl chloroformate (77.6 mg, 0.49 mmol) was added and the mixture was stirred for 10 minutes. Ethyl magnesiumbromide (0.589 ml, 1M in THF) was added at −30° C. and the mixture was stirred for 30 minutes, partitioned between diethylether and aqueous ammonium chloride solution, the combined organic extracts were dried over sodium chloride and evaporated to dryness in vacuo. The raw material was purified by silica gel chromatography with a heptane/ethyl acetate gradient to yield the title compound (84 mg).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08618304B2
出典データセットuspto-grants-2013_12
ORD IDord-25408ee88b57454f8d3d98a4f9bc8f07
出典メモuspto-grants-2013_12