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HRID 332571作成日:2026年10月27日

Hydrochloric Acid → 1-Fluoro-3-methoxy-2-(3-nitro-phenoxy)-benzene

https://huagongshe.com/reaction/332571

反応式

関与物質

役割名称HCID仕込み量
反応物Hydrochloric AcidHCID 313—
反応物N,N-DimethylglycineHCID 673—
反応物Cesium carbonateHCID 10796—
反応物1-Iodo-3-nitrobenzeneHCID 12574—
反応物2-Fluoro-6-methoxyphenolHCID 2737367—
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-Fluoro-3-methoxy-2-(3-nitro-phenoxy)-benzeneHCID 5770111578.7%

反応条件

温度98 °C

反応手順

To a 250 mL pressure resistant vial which contained a mixture of 2-fluoro-6-methoxy-phenol (1000 mg, 7 mmole), 1-iodo-3-nitro-benzene (2500 mg, 10 mmole), Cs2CO3 (1200 mg, 7 mmole) and N,N-dimethylglycine.HCl (200 mg, 1.5 mmole) in dioxane (40 mL) was added CuI (140 mg, 0.7 mmole) at rt. The reaction mixture was bumbled with Ar for 5 min at rt and then the vial was sealed. The reaction mixture was stirred and heated to 98° C. for 5 d. After cooling to rt, the reaction mixture was poured into 250 mL ice-water which was extracted with ethyl acetate (3×50 mL), washed with water (2×50 mL), brine (50 mL) and dried over Na2SO4. After removal of solvent, the residue was purified by silica gel column chromatography with ethyl acetate/hexane as eluent to give 1450 mg (75% yield) of product (10).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08877816B2
出典データセットuspto-grants-2014_11
ORD IDord-7d5582b738464520abf25e5d6d00ca9e
出典メモuspto-grants-2014_11