Optimization of extraction conditions and phytochemical screening of the root bark of Synadenium glaucescens were carried out in a stepwise manner in order to obtain the highest yields and the constituents of the extracts. Sequential extraction using Soxhlet method was performed using dichloromethane, hexane and petroleum ether, respectively, each followed by ethanol. Extraction conditions included: running time of 2 to 6 hours, temperature at 25 oC to 95 oC and particle size ranging from 0.4 mm to> 3mm diameter. Phytochemical screening was done using derivatisation techniques, gas chromatography-mass spectrometry and high performance liquid chromatography. Extraction with dichloromethane followed by ethanol resulted in a higher yield by 25%, within 4 hrs of extraction, particle size of 1mm, at temperatures of 30 oC for dichloromethane and 75 oC for ethanol. Fatty acid analysis indicated absence of free fatty acids in both Dichloromethane and ethanolic extracts. Silylation and Thin Layer Chromatography indicated the presence of non hindered and hindered functionality and the presence of triterpenoids in the dichloromethane extract. Phytochemical screening of the dichloromethane extracts indicated that it is composed of two main triterpenoids that best matched with Lanosterol (42%) and Cycloartenol (31%). Other minor compounds identified through chromatographic analysis were phytol, ergostadiol, hentriacontane, sitastirol aceate, lupeol and hopenone. The ethanolic extracts indicated the presence of polyphenolic compounds.