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ChemicalBook CAS DataBase List Methyl 4'-bromomethyl biphenyl-2-carboxylate

Methyl 4'-bromomethyl biphenyl-2-carboxylate synthesis

13synthesis methods
114772-34-8 Synthesis
4′-Methylbiphenyl-2-carboxylic acid methyl ester

114772-34-8
284 suppliers
$12.00/1g

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Yield:114772-38-2 96.2%

Reaction Conditions:

with tetrabutylammonium bromide;dihydrogen peroxide;bromine in diethyl ether at 60; for 2.5 h;

Steps:

5-7

45.3g (0.2mol) of methyl 4'-methyl-2-biphenylcarboxylate was added to 275g of n-hexane, then 36.3g (0.204mol) of NBS and 1.64g (0.01mol) of AIBN were added, and the temperature was raised to At 60°C, 45.4g (0.4mol) of 30% hydrogen peroxide was added dropwise, the dropping was completed in about 2h, the temperature was raised to reflux for 30min, and the residual raw material was controlled by HPLC to be ≤1.0%; cooled to ≤30°C, 10% was added dropwise Sodium bisulfite solution 70g, dripped, stirred for 30min, filtered, the filter cake was rinsed with 150g of n-hexane, the filter cake was dried,58.8 g of ethyl 4'-bromomethyl-2-biphenylcarboxylate (white solid) was obtained, with a molar yield of 96.2%, HPLC: 99.54%, and no dibromo impurity was detected.

References:

CN114436833,2022,A Location in patent:Paragraph 0051; 0053-0054; 0056-0057; 059

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