2,6-Di-tert-butyl-4-methylphenol → 3-[4-[2-(N-Dodecyl-N-methylamino)ethoxy]-2-vinylphenyl]propanoic acid, methyl ester

温度

100 °C

To a solution of 3-[4-[2-(N-dodecyl-N-methylamino)ethoxy]-2-[trifluoromethanesulfonyloxy]-phenyl]propanoic acid, methyl ester (250 mg, 0.48 mmol) in 1,4dioxane (2.5 ml) were added tributylvinyltin (1.2 ml, 4.0 mmol), lithium chloride (123 mg, 1.44 mmol), tetrakis(triphenylphosphine)-palladium(0) (10 mg) and 2,6-di-tert-butyl-4-methylphenol (10 mg). The resulting mixture was then stirred at 100° C. for 5 h. After cooling to r.t., the mixture was diluted with diethyl ether, washed with water, brine, dried over magnesium sulfate and concentrated in vacuo. The residue was chromatographed on silica gel (diethyl ether/acetone 100:0 to 80:20) to afford the title compound (170 mg, 80%) as a yellow oil.

1. temperatureAfter cooling to r.t.
2. washwashed with water, brine
3. dry with materialdried over magnesium sulfate
4. concentrationconcentrated in vacuo
5. customThe residue was chromatographed on silica gel (diethyl ether/acetone 100:0 to 80:20)

ORDレコード

ord-0fd06fd682b64d01bbb41414cd9da783

出典データセット

uspto-grants-2001_07

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06255496B1