Rapid synthesis of Gemini surfactants (C(12)-C(2)-C(12) and C(14)-C(6)-C(14)) by microwave heating is investigated. The yield of the synthesis of C(12)-C(2)-C(12) surfactant using 2.45-GHz microwaves was twice the yield obtained by the oil bath method. Moreover, the value of dielectric loss and microwave penetration depth for the sample solution suggest that the microwave frequency of 915 MHz (0.915 GHz) is preferable over the conventional frequency (2.45 GHz). A novel 915-MHz microwave organic synthesis apparatus with a closed reactor is proposed. The synthesis yields of C(12)-C(2)-C(12) obtained using the 915-MHz equipment were three to four times higher than those obtained using the conventional heating method.