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Prepn. of chlorinating reagent or chlorination reaction itself for use in a reaction such as prodn. of high intensity sweetener trichlorogalactosucrose (TGS) from partially protected sucrose comprising reaction of DMF with thionyl chloride or another sulfur contg. inorg. acid chlorides including sulfuryl chloride is faced with a problem of prolific release of gaseous byproducts, that at times may lead to violent explosion also.  This problem is solved by innovative addn. of solid powder inert to the constituents of the chlorination reaction mixt. to the reaction, or by adding DMF to acid chloride soln. in that order.  The invention also leads to use of isolated solid Vilsmeier reagent being used for chlorination in a solvent other than DMF making it possible to avoid altogether problems arising from use of DMF which include irrecoverable loss in alk. as well as acid conditions, interference in crystn. of TGS and the like.

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