A reactor setup consisting of two stainless steel microreactors [gas-phase microreactor (GPMR)-mix from the Institut für Mikrotechnik Mainz (IMM)] coupled in series was used for production of methyl chloride by hydrochlorination of methanol. The catalyst was γ-alumina on microreactor platelets. The influence of temperature on the methanol conversion and methyl chloride selectivity was investigated. A maximum conversion of 97.6% and a selectivity of 98.8% were reached at 340°C, which is close to the calculated thermodynamic equilibrium. Comparison with results obtained from a single microreactor and the modified setup of two microreactors revealed that the serial coupling resulted in a dead volume with a blind activity, which cannot be neglected when describing the setup. Furthermore, the separation of methyl chloride using condensers was investigated. The proposed microreactor-condenser concept enables the production of methyl chloride with a high purity.