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HRID 625696作成日:2026年10月25日

Triethylamine → Methyl 3-(2-bromo-3,5-difluorophenyl)propanoate

https://huagongshe.com/reaction/625696

反応式

関与物質

役割名称HCID仕込み量
反応物TriethylamineHCID 8471—
反応物Acrolein dimethyl acetalHCID 80145—
反応物1,2-Dibromo-3,5-difluorobenzeneHCID 2724517—
触媒Tetrabutylammonium ChlorideHCID 70681—
溶媒DimethylformamideHCID 6228—
生成物Methyl 3-(2-bromo-3,5-difluorophenyl)propanoateHCID 89826041—

反応条件

温度90 °C

反応手順

A mixture of 1,2-dibromo-3,5-difluorobenzene (4.5 g), 3,3-dimethoxyprop-1-ene (5.1 mL), tetrabutylammonium chloride (4.6 g) and triethylamine (3.5 mL) in N,N-dimethylformamide (50 mL) is purged with nitrogen for 20 minutes. Palladium-(II)-acetate (111 mg) is added and the mixture heated for 16 hours at 90° C. After cooling the mixture is partitioned between aqueous HCl (1 M) and diethyl ether, the organic layer dried (Na2SO4), volatiles evaporated under reduced pressure and the residue purified by column chromatography (silica gel; hexane:ethyl acetate 98:2→80:20) to give the title compound (Yield 3.6 g).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US09308194B2
出典データセットuspto-grants-2016_04
ORD IDord-8f53b8bc5e954936a05f94d1a5e40149
出典メモuspto-grants-2016_04