3,5-DibroMo-4-Methoxy-pyridine synthesis
- Product Name:3,5-DibroMo-4-Methoxy-pyridine
- CAS Number:25813-24-5
- Molecular formula:C6H5Br2NO
- Molecular Weight:266.92
67-56-1
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2457-48-9
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$43.79/250mg
25813-24-5
51 suppliers
$15.00/250mg
Yield:25813-24-5 95%
Reaction Conditions:
Stage #1:methanol with sodium hydride in tetrahydrofuran at 0; for 0.25 h;
Stage #2:3,4,5-tribromopyridine in tetrahydrofuran at 20; for 19 h;
Steps:
31
To a solution of MeOH (0.115 mL, 2.85 mmol) and THF (0.5 mL) at 0 °C was added sodium hydride (60% dispersion, 1 14 mg, 2.85 mmol). After stirring for 15 min, Intermediate 3 IB (600 mg, 1.900 mmol) was added, and the resulting mixture was stirred at room temperature for 19 hours, diluted with water (3 mL) and extracted with EtOAc (2 x 10 mL). The combined organics were washed with brine, dried over anhydrous sodium sulfate, and concentrated under reduced pressure to yield Intermediate 31 (0.480 g, 1.798 mmol, 95% yield) as a beige color solid. MS (ES): m/z=267.9 [M+H]+. XH NMR (400 MHz, MeOD) δ ppm 8.68 (2 H, s), 3.99 (3 H, s).
References:
BRISTOL-MYERS SQUIBB COMPANY;AUSTIN, Joel, Francis;SHARMA, Lisa, S.;BALOG, James, Aaron;HUANG, Audris;VELAPARTHI, Upender;DARNE, Chetan, Padmakar;SAULNIER, Mark, George WO2012/15723, 2012, A1 Location in patent:Page/Page column 93
25813-25-6
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124-41-4
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$12.00/25g
25813-24-5
51 suppliers
$15.00/250mg
13626-17-0
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$5.00/100mg
124-41-4
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$12.00/25g
25813-24-5
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$15.00/250mg
25813-25-6
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$29.00/1g
74-88-4
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$15.00/10g
25813-24-5
51 suppliers
$15.00/250mg
626-64-2
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$6.00/5g
25813-24-5
51 suppliers
$15.00/250mg