2-broMo-4'-broMoMethylacetophenone synthesis

Yield:62546-51-4 87%

Reaction Conditions:

with N-Bromosuccinimide;tetrachlorosilane in acetonitrile at 20; for 6 h;

Steps:

Typical procedure for the halogenations of 1 or 6 with SiCl₄/NXS

General procedure: To a mixture of NXS and substrate (1 or 6) in CH₃CN at room temperature was added SiCl₄ and the mixture left to stir until TLC showed the disappearance of the starting material. The reaction was then poured onto H₂O and the mixture extracted with CH₂Cl₂. The extracts were combined, dried over MgSO₄ and evaporated. The residue was purified by recrystallization (pet. ether-Et₂O, 3:1) to give pure 2b-2g, 3b, or by silica gel column chromatography (hexane-EtOAc 10:1 or 30:1) to give pure 2a,h,i, 3a-5 or 7-9, respectively

References:

Salama, Tarek A.;Novák, Zoltán [Tetrahedron Letters,2011,vol. 52,# 31,p. 4026 - 4029] Location in patent:experimental part