A process of producing a methylphenyltrisiloxane having the following general formula: ##STR1## wherein R.sup.1 and R.sup.2 may be the same or different and are each a methyl or phenyl group, the process comprising the step of reacting: (A) methyldiphenylsilanol, with (B) a silazane compound having a diorganosilazane unit having the following formula: ##STR2## wherein R.sup.1 and R.sup.2 are as defined above. According to the process, colorless and odorless methylphenyltrisiloxanes can be obtained easily, safely and economically, without any special deodorizing or decoloring step.