We have studied the kinetics of the chemical reaction between Mg and B by differential thermal analysis. There are two exothermal peaks observed at 500 and 650 °C. We speculate that the first exothermal peak is mainly related to the chemical reaction between Mg and oxygen, forming MgO. The second exothermal peak, which coincides with the melting point of Mg, clearly indicates the chemical reaction between Mg and B. The effect of synthesis conditions and defects on the transport property of MgB2 has been investigated. A correlation between the microstrain, the lattice parameters, and the Mg concentration were observed and are discussed.