Due to the explosive nature of H2,O2and CH4mixtures, the concept of couplingin situsynthesis of H2O2with low-temperature single-step methane conversion to methanol has not received sufficient attention.This study aimed to investigate this process using a microchannel reactor, which offers the opportunity toexplore the process under a wide range of concentrations. Direct methane activation within situgenera-tion of H2O2was successfully demonstrated in a microcapillary containing Au–Pd nanoparticles embeddedon its silica-coated walls. The effect of H2,O2and CH4partial pressures, H2/O2molar ratio, gas-to-liquid(G/L) ratio and liquid phase weight-hourly-space-velocity (WHSV) on the productivity and product distribu-tion was investigated. CH4partial pressure had the most significant effect on the productivity, while H2andO2partial pressures influenced the productivity less. The methane activation rate was found to be corre-lated with the H2O2formation rate. With only O2or pre-formed stabilized H2O2methane activation wasnot found,in situH2O2synthesis was therefore essential. G/L affected neither the product distribution northe productivity, however, lowering WHSV altered the product distribution favoring methanol formation.