ChemicalBook CAS DataBase List 2,6-Dichloroisonicotinic acid

2,6-Dichloroisonicotinic acid synthesis

11synthesis methods

Product Name:2,6-Dichloroisonicotinic acid
CAS Number:5398-44-7
Molecular formula:C6H3Cl2NO2
Molecular Weight:192

99-11-6 Synthesis

99-11-6
254 suppliers
$11.00/10g

5398-44-7
322 suppliers
$6.00/1g

Yield:5398-44-7 89%

Reaction Conditions:

with tetraethylammonium chloride;trichlorophosphate at 130 - 145; for 20 h;

Steps:

16 Example 16-2,6-dichloroisonicotinic acid
Citrazinic acid (10.35 g, 66.7 mmol) and tetraethylammonium chloride (11.05 g, 66.7 mmol) were suspended in phosphoroxychloride (20 mL, excess) and heated at 130 °C for 18 h and then at 145 °C for 2 h. The reaction mixture was allowed to cool to RT and poured onto crushed ice (150 g). Extraction of ethyl acetate (3 x 100 mL), drying of the combined organic layers (MGS04) and evaporation in vacuo gave 11. 34 g (89 %) of a white solid. IH NMR (400 MHz, DMSO-d6) 8 7.85 (s, 2H) 13.90 (br s, OH).

References:

BIOVITRUM AB WO2004/63156, 2004, A1 Location in patent:Page 35

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