A new protocol for the methylation of aryl halides using the AlMe3 analogue DABAL-Me-3 in a VOC/IL biphasic system is described. Very good isolated yields and chemoselectivities (methylation vs homocoupling), were observed in alkylmethylimidazolium and DABCO-based ILs, in presence of a bulky substituted phosphine (XPhos) and the structurally related sulfonated phosphine (XPhosSO(3)H). Recycling experiments of the IL-catalyst systems were satisfactory only in case of the butyldimethylimidazolium IL due to catalyst loss to the VOC phase. (C) 2010 Elsevier B.V. All rights reserved.