OTAVA-BB BB7018670077 synthesis
- Product Name:OTAVA-BB BB7018670077
- CAS Number:773865-48-8
- Molecular formula:C11H8INO3
- Molecular Weight:329.09
951006-39-6
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773865-48-8
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$204.00/1g
Yield:-
Reaction Conditions:
Stage #1: ethyl 6-iodo-8-methyl-4-oxo-1,4-dihydroquinoline-3-carboxylatewith sodium hydroxide;water in ethanol; for 1 h;Heating / reflux;
Stage #2: with hydrogenchloride in ethanol;water; pH=2;
Steps:
3
Ethyl 6-iodo-8-methyl-4-oxo-1 ,4-dihydro-3-quinolinecarboxylate (155g) (Intermediate 2) was suspended in a mixture of ethanol (445ml) and 2M sodium hydroxide (870ml), and the mixture was heated under reflux for 1 h. The solution was cooled, the solvent reduced to low volume (400ml removed), and the pH was adjusted to ca. pH 2 with concentrated hydrochloric acid {ca. 150ml) with cooling. A solid separated, which was washed with water, and dried at 40° under vacuum to give the title compound as a white solid (139g). 1 H NMR (400 MHz, DMSO-Cf6) δ ppm 2.55 (s, 3 H) 8.08 (s, 1 H) 8.40 (s, 1 H) 8.62 (s, 1 H) 12.77 (s, 1 H) 15.02 (s, 1 H).
References:
WO2007/107499,2007,A1 Location in patent:Page/Page column 22
13194-68-8
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$6.00/1g
773865-48-8
29 suppliers
$204.00/1g
951006-38-5
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773865-48-8
29 suppliers
$204.00/1g