Trimethylsilylacetylene → 2,2,2-Trifluoro-N-{2-fluoro-5-[(trimethylsilyl)ethynyl]phenyl}acetamide

温度

60 °C

To an oven-dried flask under N2 was added N-(5-bromo-2-fluorophenyl)-2,2,2-trifluoroacetamide (5.6 g, 20 mmol), anhydrous degassed THF (200 mL), dichlorobis(triphenylphosphine)palladium(II) (1.7 g, 2.5 mmol), copper(I) iodide (0.28 g, 1.5 mmol), and trimethylsilylacetylene (7.0 mL, 50 mmol). Next, TEA (27 mL, 197 mmol) was added dropwise and the resulting mixture was heated at 60° C. overnight. The crude reaction mixture was adsorbed to silica gel and purified by column chromatography to afford the desired product (5.3 g, 89%) as an off white solid. ES-LC/MS m/z=302 [M−H]−.

1. customThe crude reaction mixture
2. custompurified by column chromatography

ORDレコード

ord-2bf5e49314df42a89302567b4e61fa5c

出典データセット

uspto-grants-2010_10

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07807673B2