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Biodiesel is a domestically produced renewable fuel that can be manufactured from vegetable oils, such as palm oil, for use in diesel vehicles.. In this research, the biodiesel was synthesized from palm oil mill effluent using co-solvent diethyl ether to observe its effect on decreasing the yield of biodiesel. In other hand, it was synthesized using calcium oxide (CaO) as a heterogeneous catalyst. Biodiesel has been made systematically by reacted oil, methanol, co-solvent diethyl ether, and sulfuric acid as catalyst in esterification process, calcium oxide on transesterification. Each reaction using various of co-solvent ratio : triglyceride (palm oil mill effluent) (CPO:DEE) 1:0,5., 1:1., dan 1:1,5 b/v, and catalyst ratio are CaO 3%, 6%, dan 8% b/b. The optimum transesterification conditions to obtain the 59,82% yield of biodiesel are as follows: CPO/DEE 1:0,5 b/v and 8 wt.% catalyst , with biodiesel yields of 59,82%. The highest yield of the effect ratio co-solvent diethyl ether on 1:1,5 b/v, 8 wt.% catalyst was 69,045%. The infrared spectra showed the absorption of ester functional groups. It was supported by GC-MS data that showed the formation of methyl ester: methyl palmitate (42,08%), methyl oleate (36,27%), methyl linoleate (12,78%), dan methyl stearate (6,04%). The physical characteristics of biodiesel are density, viscosity, Free Fatty Acid value, moisture content, iodine value, saponification number, and cetane number,: 0,825 g/cm3, 4,792 cSt, 0,8 mgNaOH/g biodiesel, 0,598% weight, 28,52 gI2/g biodiesel, 147,31 gKOH/g biodiesel, and 76,03 for cetane number, respectively.