2,5,6-Trichloropyridine-3-carboxamide → 2,5,6-Trichloronicotinonitrile

Temperatur

90 °C

A suspension of 2,5,6-trichloronicotinamide (Method 45, 2.3 g, 10.2 mmol) in POCl3 (20 ml) was heated to 90° C. for 1 hour. The reaction was then cooled to room temperature, and the POCl3 was removed under vacuum. The resulting residue was taken up in DCM (50 ml) and ice water (50 ml) was then added, followed by the careful addition of an aqueous solution of Na2CO3 until pH 8 was achieved. The organic fraction was then dried over Na2SO4, filtered, and concentrated to give the title compound (2.1 g, 80%) which was used without further purification. 1H NMR (400 MHz, CD3OD) δ 8.54 (s, 1H).

1. temperatureThe reaction was then cooled to room temperature
2. customthe POCl3 was removed under vacuum
3. additionice water (50 ml) was then added
4. additionfollowed by the careful addition of an aqueous solution of Na2CO3 until pH 8
5. dry with materialThe organic fraction was then dried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated

ORD-Eintrag

ord-edd9523f33944804b58d0ae1af88185f

Quelldatensatz

uspto-grants-2012_12

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08324252B2