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ChemicalBook CAS DataBase List 2-Pyridinecarboxylic acid, 5,6-dichloro-

2-Pyridinecarboxylic acid, 5,6-dichloro- synthesis

3synthesis methods
-

Yield: 75%

Reaction Conditions:

with trichlorophosphate at 0 - 95; for 1 h;

Steps:

83.a
The colorless oil, 5-chloro-1-oxy-pyridine-2-carboxylic acid (1.2 g, 7 mmol) was added into POCl3 (10 g) at 0° C. and the mixture was heated to 95° C. for 1 h. The reaction mixture was evaporated to dryness. The residue was dissolved in 15 mL water and extracted with ethyl acetate (2×15 mL), the combined organic layer was washed with water (2×30 mL) and brine (30 mL), then evaporated to dryness to obtain the title compound (1 g, 75%) as a yellow solid, MS (EI): m/e=191.9 [M+H]+.

References:

Bissantz, Caterina;Grether, Uwe;Hebeisen, Paul;Kimbara, Atsushi;Liu, Qingping;Nettekoven, Matthias;Prunotto, Marco;Roever, Stephan;Rogers-Evans, Mark;Schulz-Gasch, Tanja;Ullmer, Christoph;Wang, Zhiwei;Yang, Wulun US2012/316147, 2012, A1 Location in patent:Page/Page column 66