2,6-Dichloronicotinoyl chloride synthesis

Yield:58584-83-1 100%

Reaction Conditions:

with thionyl chloride in chloroform;N,N-dimethyl-formamide; for 17 h;Reflux;

Steps:

3.3.1

Example 3; 2-Amino-1-ethyl-4-oxo-7-[4-(3-pyridin-3-ylmethylureido)phenyl]-1,4-dihydro[1,8]naphthyridine-3-carboxylic Acid Ethyl Ester (No. 10)3.1: 2,6-dichloronicotinic Acid Chloride58 ml (0.796 mmol) of thionyl chloride are added, dropwise, to a suspension of 30.58 g (0.159 mmol) of 2,6-dichloronicotinic acid in 200 ml of chloroform and 0.1 ml of DMF, and then the mixture is refluxed for 17 hours. The mixture is allowed to return to ambient temperature and then the solvent is evaporated off under reduced pressure. The residue obtained is taken up in toluene and evaporated to dryness. 33.53 g of an amber liquid are obtained. The yield is quantitative.

References:

US2011/251194,2011,A1 Location in patent:Page/Page column 15