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HRID 642747作成日:2026年10月25日

Potassium Phosphate, Tribasic → 1-(3-Chloro-4-cyano-2-methylphenyl)-2-oxo-octahydrocyclopenta[b]-pyrrol-4-yl benzoate

https://huagongshe.com/reaction/642747

反応式

関与物質

役割名称HCID仕込み量
反応物Potassium Phosphate, TribasicHCID 62657—
反応物2-Chloro-4-iodo-3-methylbenzonitrileHCID 16731995—
反応物1-Oxo-octahydrocyclopenta[c]pyrrol-4-yl benzoateHCID 59259560—
反応物2-Oxo-octahydrocyclopenta[b]pyrrol-4-yl benzoateHCID 59259571—
触媒Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)HCID 24350—
溶媒1,4-DioxaneHCID 31275—
生成物1-(3-Chloro-4-cyano-2-methylphenyl)-2-oxo-octahydrocyclopenta[b]-pyrrol-4-yl benzoateHCID 59259566—
生成物2-(3-Chloro-4-cyano-2-methylphenyl)-1-oxo-octahydrocyclopenta[c]-pyrrol-4-yl benzoateHCID 59259573—

反応条件

温度110 °C

反応手順

To a vial containing mixtures of compound 1I and 1J (100 mg, 0.4 mmol) obtained from previous step in dioxane (1 mL) were added CuI (15.6 mg, 0.08 mmol), K3PO4 (174 mg, 0.82 mmol), 1,2-cyclohexyldiamine (4.7 mg, 0.08 mmol) and compound 1E (136 mg, 0.49 mmol). The vial was sealed, and heated at 110° C. for 14 hr, cooled to RT. The solid was filtered off, and filtrate was concentrated. Purification by silica gel chromatography (5% to 100% EtOAc in hexanes, then 10% methanol in EtOAc) provide the mixtures of title compounds 1K and 1L (total 98 mg) as a yellow oil. MS (ES) m/z 395 [M+H]+.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07696241B2
出典データセットuspto-grants-2010_04
ORD IDord-722b3a5356f24a2ab6d966e77bcf9ecd
出典メモuspto-grants-2010_04