Chloride → Ethyl 3-chloro-4-trifluoromethylcinnamate

Temperatur

140 °C

A suspension of 3.5 g of 2,4-dichlorobenzotrifluoride, 1.28 g of triphenylphosphine, 865 mg of paradium(II) chloride, 2.68 g of sodium iodide, 712 mg of nickel(II) bromide, 4.94 g of triethylamine, and 1.79 g of ethyl acrylate in 16 ml of N,N-dimethylformamide was heated at 140° C. for over night in a sealed tube. The reaction mixture was filtrated off, and the filtrate was concentrated under a reduced pressure. The residue was extracted with ethyl acetate, the extract was washed with water, dried, and evaporated under a reduced pressure. The resulting residue was purified by a silica gel column chromatography to give 1.12 g of ethyl 3-chloro-4-trifluoromethylcinnamate.

1. filtrationThe reaction mixture was filtrated off
2. concentrationthe filtrate was concentrated under a reduced pressure
3. extractionThe residue was extracted with ethyl acetate
4. washthe extract was washed with water
5. customdried
6. customevaporated under a reduced pressure
7. customThe resulting residue was purified by a silica gel column chromatography

ORD-Eintrag

ord-6626cf1b872c47869f0e7a6cb26ae6f8

Quelldatensatz

uspto-grants-1994_03

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US05294718