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ChemicalBook CAS DataBase List METHYL 2-BROMO-3-NITROBENZOATE

METHYL 2-BROMO-3-NITROBENZOATE synthesis

7synthesis methods
-

Yield:5337-09-7 100%

Reaction Conditions:

with sodium carbonate in N,N-dimethyl-formamide at 60; for 4 h;

Steps:

36.a (a) methyl 2-bromo-3-nitrobenzoate
(a) methyl 2-bromo-3-nitrobenzoate To a solution of 2-bromo-3-nitrobenzoic acid (33.9 g, 138 mmol) in DMF (240 mL) were added Na2C03 (58.5 g, 552 mmol) and iodomethane (34 mL, 544 mmol). The reaction mixture was heated at 60 °C for 4 h. The reaction mixture was diluted with water (1.5 L) and extracted with Et20 (2 x 750 mL). The combined organic layers were washed with brine (500 mL) and concentrated to afford methyl 2-bromo-3-nitrobenzoate (36.78 g, 137 mmol, 100% yield) as a yellow solid. LC-MS (ES) m/z = 259.9, 261.9 [M+H]+.

References:

GLAXOSMITHKLINE INTELLECTUAL PROPERTY (NO.2) LIMITED;KNIGHT, Steven David;LAFRANCE, Louis Vincent III;MCNULTY, Kenneth C.;ROMERIL, Stuart Paul;SEEFELD, Mark Andrew WO2014/195919, 2014, A1 Location in patent:Page/Page column 157

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