Propargyl alcohol → HCID 59407577, Verbindung

A mixture of 1-iodo-3-(trifluoromethoxy)benzene (5.00 g), copper(I) iodide (66.3 mg), triphenylphosphine (228 mg), tris(dibenzylideneacetone)dipalladium(0) chloroform adduct (360 mg), propargyl alcohol (1.13 ml), diisopropylethylamine (12.1 ml) and tetrahydrofuran (100 ml) was stirred at room temperature for 15 hr. The reaction mixture was added to brine, and the mixture was extracted with ethyl acetate, washed with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=100:0-80:20) to give the object product (3.28 g) as a brown oil.

1. extractionthe mixture was extracted with ethyl acetate
2. washwashed with saturated brine
3. dry with materialdried over anhydrous magnesium sulfate
4. customThe solvent was evaporated under reduced pressure
5. customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=100:0-80:20)

ORD-Eintrag

ord-7617013fcc0c40068a911a7fa1860f87

Quelldatensatz

uspto-grants-2012_03

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08129361B2