METHYL 5-BROMO-6-HYDROXYNICOTINATE synthesis
- Product Name:METHYL 5-BROMO-6-HYDROXYNICOTINATE
- CAS Number:381247-99-0
- Molecular formula:C7H6BrNO3
- Molecular Weight:232.03
66171-50-4
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$12.00/1/ G
381247-99-0
95 suppliers
$17.00/250mg
Yield:381247-99-0 100%
Reaction Conditions:
Stage #1: methyl 6-hydroxynicotinatewith bromine;acetic acid at 60;
Stage #2: with sodium hydrogencarbonate;sodium hydroxide at 18 - 26; pH=~ 7;
Steps:
117
Intermediate 117Methyl 5-bromo-6-hvdroxynicotininate Methyl 6-hydroxynicotininate (Intermediate 116, 50 g, 327 mmol) was suspended in acetic acid (250 mL) and bromine (26.2 mL, 490.5 mmol) was added dropwise to the reaction. The reaction was then heated at 6O0C for 18 h. The reaction mixture was cooled to room temperature, and saturated sodium thiosulfate solution was added to remove remaining bromine. Saturated sodium bicarbonate solution (500 mL) was added slowly, then IN sodium hydroxide was added carefully until the pH was ~7. The solid that precipitated were collected by filtration and dried in a vacuum oven at 50°C for 18 h. This gave 76g (100%) of methyl 5- bromo-6-hydroxynicotininate as an off white solid. MS (ESP): 231.9(MH+) for C7H6BrNO3
References:
WO2009/106885,2009,A1 Location in patent:Page/Page column 296-297
67-56-1
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41668-13-7
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$13.00/1g
381247-99-0
95 suppliers
$17.00/250mg
5006-66-6
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381247-99-0
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$17.00/250mg
42933-07-3
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$11.00/100mg
381247-99-0
95 suppliers
$17.00/250mg
67-56-1
803 suppliers
$9.00/25ml
381247-99-0
95 suppliers
$17.00/250mg