Procarbazine, an important API (active pharmaceutical ingredient) is present in many commercial anticancer drugs like Matulane (USA), Natulan (Canada) and Indicarb (India). In this paper, the authors report a procedure for the synthesis of the key intermediate dibenzyl 1-[4-(isopropylcar-bamoyl)benzyl]-2methylhydrazine-l,2-dicarboxylate (5) including 5 steps starting from methylhydrazine and methyl 4(hydroxymethyl) benzoate which are easily-available chemicals. The total yield of the key intermediate is about 50 percent, related to the starting materials.