5-Bromo-6-chloronicotinic acid synthesis
- Product Name:5-Bromo-6-chloronicotinic acid
- CAS Number:29241-62-1
- Molecular formula:C6H3BrClNO2
- Molecular Weight:236.45
41668-13-7
165 suppliers
$13.00/1g
29241-62-1
236 suppliers
$5.00/250mg
Yield:29241-62-1 97%
Reaction Conditions:
Stage #1:5-bromo-6-hydroxy-3-pyridinecarboxylic acid with tetramethlyammonium chloride;trichlorophosphate for 3 h;Heating / reflux;
Stage #2: with water at 0; for 2 h;
Steps:
8.B
8B. 5-Bromo-6-chloro-nicotinic acid: To 8A (10 g, 45 mmol) was added tetra-methylammonium chloride (5.4 g, 49 mmol) and phosphorous oxychloride (20 mL) and the reaction was heated at reflux for 3 h. The reaction was poured onto ice and stirred 2 h. The solid was filtered off, dissolved in EtOAc (300 mL) and dried (Na2SO4). After filtration and concentration, 10.5g (97%) of 8B as a pink solid was collected. 1HNMR (400 MHz, DMSO-d6) δ: 8.53 (d, J = 2.02 Hz, 1H) 8.85 (d, J = 2.02 Hz, 1 H) 13.57 (s, 1 H).
References:
BRISTOL-MYERS SQUIBB COMPANY WO2007/70818, 2007, A1 Location in patent:Page/Page column 103
17282-03-0
219 suppliers
$10.00/1g
29241-62-1
236 suppliers
$5.00/250mg
5006-66-6
470 suppliers
$13.43/1gm:
29241-62-1
236 suppliers
$5.00/250mg
5006-66-6
470 suppliers
$13.43/1gm:
29241-62-1
236 suppliers
$5.00/250mg