A representative series of (organoethynyl) difluoroboranes RCCBF2 (RC4H9,(CH3) 3C, CF3, C3F7,(CF3) 2CF, CF3CFCF, C4F9CFCF, C6F5) was prepared by abstraction of fluoride from the corresponding K [RCCBF3] salts with BF3 in appropriate solvents (1, 1, 1, 3, 3-pentafluoropropane, 1, 1, 1, 3, 3-pentafluorobutane, or dichloromethane).