Trichloroacetyl chloride → 2,2,2-Trichloro-N-(pyridin-3-YL)acetamide

To a solution of 3-aminopyridine (1.0 g, 11 mmol) and triethylamine (1.3 g, 13 mmol) in tetrahydrofuran (30 mL) was added at 0° C. trichloroacetyl chloride (1.4 mL, 13 mmol), and the mixture was stirred at 0° C. for 20 minutes. The reaction solution was concentrated, and ethyl acetate was added to the residue. The resulting mixture was washed with water and saturated brine and dried over magnesium sulfate. The solid was filtered off, and the filtrate was concentrated. The residue was washed with diisopropyl ether and collected by filtration to obtain the title compound (2.3 g, yield 89%) as colorless powder.

1. concentrationThe reaction solution was concentrated
2. additionethyl acetate was added to the residue
3. washThe resulting mixture was washed with water and saturated brine
4. dry with materialdried over magnesium sulfate
5. filtrationThe solid was filtered off
6. concentrationthe filtrate was concentrated
7. washThe residue was washed with diisopropyl ether
8. filtrationcollected by filtration

ORD-Eintrag

ord-7108aa33f66d415fb6c6ff0ecef25837

Quelldatensatz

uspto-grants-2010_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07795267B2