N-(2,3-Dimethyl-phenyl)-N′-(methoxyl formyl)thiourea was synthesized by the reacting of 2,3-dimethy-laniline,potassium thiocyanate(KSCN)and methyl chloroformate(C1COOCH3).Single crystal was obtained by slowly evaporation solvent at room temperature.The structure was characterized by elemental analysis,IR and X-ray crystalography.The compound crystallized:a triclinic system with space group P(i),a=0.83440(12)nm,b=0.89113(13)nm,c=0.93015(13)nm,a=76.548(2)°,β=63.906(2)°,γ=82.538(2)°,V=0.60379(15)nm3,Z=2,Dc=1.311 mg/m3,F(000)=252,μ=0.256 mm-1,R1=0.0379,wR2=0.0919.The specific heat capacity of the title compound was determined by a Micro-DSC method,and the specific heat capacity was 1.25 J·g-1·K-1 at 298.15 K.Thermodynamic functions,relative to those at the standard temperature of 298.15 K,were calculated via thermodynamic relationship.The thermal behavior of the title compound under a non-isothermal condition was studied by differential scanning calorimetry/thermogravimetric(DSC/TG)method.There was an obvious endothermic peak in the DSC curve,the peak temperature was 479.43 K.The compound mass loss was 89.94％ observed from the TG curve.