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ChemicalBook CAS DataBase List 2-(BroMoMethyl)-5-fluoro-1,3-diMethylbenzene
200799-19-5

2-(BroMoMethyl)-5-fluoro-1,3-diMethylbenzene synthesis

2synthesis methods
-

Yield:200799-19-5 34%

Reaction Conditions:

with hydrogen bromide in acetic acid at 20; for 4 h;

Steps:

67

A mixture of Scheme 60 compound 1 (5.0 g, 40.32 mmol), paraformaldehyde (15.0 g) and HBr (33% in acetic acid, 35 mL) in acetic acid (25 mL) was stirred at RT for 4 h. After TLC showed the starting material was completely consumed, the reaction mixture was diluted with water (30 mL) and extracted with petroleum ether (2 x 40 mL) then dried over Na2S04, filtered and concentrated under reduced pressure to give a residue which was purified by flash chromatography on silica gel (eluting with petroleum ether/EtOAc 100/0 gradually increasing to 90/10) to give Scheme 60 compound 2 (3.0 g, 34%) as an off-white solid. MS [ESI, MH+] = 217.99.

References:

WO2014/52365,2014,A1 Location in patent:Page/Page column 310

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