ChemicalBook CAS DataBase List 2,5,6-tetrachloropyridine

2,5,6-tetrachloropyridine synthesis

5synthesis methods

Product Name:2,5,6-tetrachloropyridine
CAS Number:54718-39-7
Molecular formula:C6H2Cl3NO2
Molecular Weight:226.44

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Yield:54718-39-7 18%

Reaction Conditions:

Stage #1: 2,5,6-trichloro-3-methylpyridinewith potassium permanganate in water at 100; for 60 h;
Stage #2: with hydrogenchloride in water at 0; pH=1 - 2;

Steps:

47

2,5,6-Trichloronicotinic acid A suspension of 2,3,6-trichloro-5-methylpyridine (Method 48, 11.8 g, 60.0 mmol) in water (400 ml) was heated to 100 ⁰C. Portionwise, KMnO₄ (28.5 g, 180.2 mmol) was then added over 12 hours. The reaction was then allowed to stir for 2 days at 100 ⁰C, over which time an additional 1O g of KMnO₄ was added portionwise. When no starting material EPO remained, the hot reaction was filtered, washed with hot water (2 x 75 ml), and the resulting filtrate was allowed to cool to room temperature. The aqueous filtrate was then extracted with EtOAc (3 x 100 ml), and then concentrated to a 50 ml volume. This aqueous solution was then cooled to 0 ⁰C and adjusted to pH 1-2 with 6.0 M HCl. The resulting solid was then collected by filtration, washed with cold water, and dried to give the title compound (2.5 g, 18%) that was used without further purification.

References:

WO2006/82392,2006,A1 Location in patent:Page/Page column 109-110

29553-51-3 Synthesis