Various acid/base compounds were used as catalysts for the synthesis of N-methyl methyl carbamate (MMC) from dimethyl urea (DMU) and dimethyl carbonate (DMC) in a batch reactor. The results showed that dibutyloxotin (DBTO) presented the best catalytic performance among the catalysts. The MMC structure was then confirmed by FTIR, 1HNMR and 13CNMR. Furthermore, effects of reaction conditions for the MMC synthesis over DBTO catalysts have been investigated. The optimal reaction conditions were as follows: DBTO 0.603 mmol，DMU 15.34 mmol, DMC 169.2 mmol, reaction temperature 423 K, reaction time 4 h, yielding MMC high to 99.96%.