A novel process is described for control of pH where acid neutralizing agents, including carbonates and bicarbonates of metals and alkaline earth metals, are used in solid form in process of large scale manufacture of a chlorinated sucrose, particularly 4,1', 6' trichlorogalactosucrose (TGS) to neutralize acidity formed when ester group containing organic solvent solutions of TGS or 6-acetyl-TGS are concentrated on a large scale. This novel method of pH control is applicable to all organic synthesis reactions where acid neutralization needs to be achieved in as much non-aqueous condition as possible. Also is described a process where use of MTBE could be used for extracting or dissolving 6-acetyl-TGS or TGS instead of ester containing organic solvents which can be concentrated without the need of pH control.