This paper presents a chemical bottom-up synthesis of highly crystalline sub micro structured metal organic framework Cu 3 (BTC) 2 (H 2 O) 3 (HKUST-1, BTC=benzene-1,3,5-tricarboxylate) prepared for the first time by a Laser ablation technique in liquid environment. The experiment consists of the ablation of a Cu metal target in a solution of DMF/H 2 O (1:1) containing benzene 1,3,5, benzene tricarboxilic acid and NaNO 3 with a high power second harmonic of a Nd:YAG laser. The X-ray and SEM measurements showed that high crystalline Cu 3 (BTC) 2 (H 2 O) 3 with octahedral morphology and dimensions in the range of 200nm to 2µm were obtained in a high yield.