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ChemicalBook CAS DataBase List METHYL 3-BROMOMETHYLPYRIDINE-2-CARBOXYLATE
116986-09-5

METHYL 3-BROMOMETHYLPYRIDINE-2-CARBOXYLATE synthesis

2synthesis methods
59718-84-2 Synthesis
METHYL 3-METHYLPYRIDINE-2-CARBOXYLATE

59718-84-2
123 suppliers
$8.00/1g

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Yield: 80.6%

Reaction Conditions:

with N-Bromosuccinimide;2,2'-azobis(isobutyronitrile) in tetrachloromethane at 90; for 16 h;Inert atmosphere;

Steps:

7.2 methyl 3-(bromomethyl)picolinate
A mixture of methyl 3-methylpicolinate (4.1 g, 27.1 mmol), NBS (5.8 g, 32.5 mmol), and AIBN (100 mg, 0.61 mmol) in carbon tetrachloride (55 mL) was stuffed at 90 °C for 16 h under nitrogen. The mixture was filtered and concentrated before being purified by column chromatography to give the desired product (5.0 g, 80.6%). ‘H NMR (400 MHz, CDC13, ): 8.67 (dd, J= 1.6, 4.6 Hz, 1 H), 7.91 (dd, J= 1.5, 7.9 Hz, 1 H), 7.48 (dd, J= 4.6, 7.9 Hz, 1 H), 4.95 (s, 2 H), 4.07 - 4.03 (m, 3 H). LCMS (mlz): 229.9 (M+1).

References:

EPIZYME, INC.;DUNCAN, Kenneth, W.;CHESWORTH, Richard;MUNCHHOF, Michael, John;SHAPIRO, Gideon WO2015/200677, 2015, A2 Location in patent:Paragraph 00472; 00473

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