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dimethyl 2-chloropyridine-3,4-dicarboxylate synthesis

3synthesis methods
3,4-Pyridinedicarboxylic acid, 3,4-dimethyl ester, 1-oxide

89663-05-8
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dimethyl 2-chloropyridine-3,4-dicarboxylate

521980-84-7
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Yield:521980-84-7 36.8%

Reaction Conditions:

with trichlorophosphate at 110;

Steps:

9.3 3) Preparation of 2-chloro-pyridine-3,4-dicarboxylic acid methyl ester

3,4-bis (methoxycarbonyl) pyridine-1-oxide (40g, 0.19mol) was added to POCl3 (400mL), and the reaction was heated to 110 deg. C overnight. A POCl3 was distilled off under reduced pressure, column chromatography (petroleum ether: ethyl acetate = 20: 1 ~ 10: 1) was isolated as the title compound (16G, yield 36.8%).

References:

CN105461714,2016,A Location in patent:Paragraph 0408; 0409; 0410