5-BROMO-2-CHLORO-N,N-DIMETHYL-3-PYRIDINECARBOXAMIDE synthesis
- Product Name:5-BROMO-2-CHLORO-N,N-DIMETHYL-3-PYRIDINECARBOXAMIDE
- CAS Number:1188142-86-0
- Molecular formula:C8H8BrClN2O
- Molecular Weight:263.52
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Yield:-
Reaction Conditions:
Stage #1: 5-bromo-2-hydroxynicotinic acidwith thionyl chloride;N,N-dimethyl-formamide at 80; for 4 h;
Stage #2: N,N-dimethylammonium chloride in dichloromethane;
Steps:
1
To a solution of compound 1 (3.0 g,) in SOCl2 (15 mL) at rt was added DMF (0.75 mL) slowly. The mixture was then refluxed at 80 °C for 4 hrs. The solvent was removed under reduced pressure and the residue was dissolved in CH2C12 (20 mL). Then the residue was dimethylamine hydrochloride (2.25 g,) was added in one portion. After addition of amine at 0 °C (11.5 mL), the reaction mixture was stirred overnight. The mixture was washed with water. The organic layer was separated and concentrated under vacuum to get desired compound 2
References:
WO2013/42035,2013,A1 Location in patent:Page/Page column 24
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