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ChemicalBook CAS DataBase List 2,3-DIFLUORO-4-METHOXYBENZYL BROMIDE

2,3-DIFLUORO-4-METHOXYBENZYL BROMIDE synthesis

1synthesis methods
-

Yield:689254-23-7 61%

Reaction Conditions:

with N-Bromosuccinimide;2,2'-azobis(isobutyronitrile) in tetrachloromethane; for 3.5 h;Heating / reflux;

Steps:

VIII

A solution of 2,3-difluoro-1-methoxy-4-nnethyl-benzene (39.5 g, 0.25 mol), N-bromo succinimide (44.5 g, 0.25 mol), and azobisisobutyronitrile (0.41 g, 2.5 mmol) in CCI4 (300 ml.) was stirred at reflux for 3.5 h. Then the formed succinimide was removed by filtration, and the filtrate was concentrated in vacuo. The residue was dissolved in Et2O (200 ml.) and concentrated to about 100 ml_. After cooling in an ice-bath the formed precipitate was filtered off, washed with cold Et2O, and dried in vacuo to give the product as a white solid. Yield: 36.O g (61%) Rf 0.3 (silica gel, petrol ether/EtOAc 20:1)

References:

WO2007/14895,2007,A2 Location in patent:Page/Page column 36; 37

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