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HRID 628474作成日:2026年10月25日

Sodium Carbonate → Ethyl 2'-chloro-4'-(trifluoromethyl)[1,1'-biphenyl]-3-acetate

https://huagongshe.com/reaction/628474

反応式

関与物質

役割名称HCID仕込み量
反応物Sodium CarbonateHCID 10340—
反応物1,4-DioxaneHCID 31275—
反応物[2-Chloro-4-(trifluoromethyl)phenyl]boronic acidHCID 2783251—
反応物Ethyl 2-(3-iodophenyl)acetateHCID 57581611—
溶媒WaterHCID 962—
生成物Ethyl 2'-chloro-4'-(trifluoromethyl)[1,1'-biphenyl]-3-acetateHCID 6697384249.6%

反応手順

Ethyl 3-iodophenylacetate (2.90 g), 2-chloro-4-(trifluoromethyl)phenyl boronic acid (3.3 g), 2M aqueous sodium carbonate solution (5 mL), dioxane (10 mL) and dichloro-bis(triphenylphosphine)palladium(II) (350 mg) were heated at 80° C. for 30 min with stirring. The reaction mixture was then cooled, poured into water, extracted with ethyl acetate, and the organic layer was separated and concentrated under vacuum in the presence of Celite® to a solid residue. This solid residue was purifed by medium pressure liquid chromatography on silica gel eluting with a gradient of ethyl acetate in hexanes to yield 1.7 g of the title compound. 1H NMR (CDCl3) δ 7.14 (s, 1H), 7.56 (d, 1H) 7.30-7.45 (m, 5H), 4.77 (q, 2H), 3.67 (s, 2H), 1.26 (t, 3H).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US09314025B2
出典データセットuspto-grants-2016_04
ORD IDord-c3372ef86a244da295e2f6154242b659
出典メモuspto-grants-2016_04