Synthesis Of 4-tert-butyl Cyclohexyl Chloroformate Of Technology By Triphosgene

4-tert-butyl cyclohexyl chloroformate is one kind of important organic intermediate, widespread uses in synthetic pesticide, medicine, spices, lead agent of chemical reagents and so on. Moreover, it is a direct material for a new synthetic peroxide initiator bis(4-tert-butylcyclohexy) peroxydicarbonate. The traditional synthesis method of 4-tert-butyl cyclohexyl chloroformate is mainly using phosgene. Phosgene, a lively gas, has been widely used in polyurethane, pesticides, pharmaceuticals, paints, dyes, triggering agent synthesis. However, phosgene is a toxic gas, it requires a high technological conditions. The operating of phosgene needs low-temperature environment, which often accompsnied with serious corrosive, prone to leskage. In addition Green Chemistry attracted more and more attentions because of it's concept in environmental beneficial synthesis. In view of these, we want develop an environmental beneficial synthesis method for synthesize 4-tert-butyl cyclohexyl choroformant without use phosgene.Purpose of this study is the use of triphosgene instead of phosgene, used in the synthesis of 4 - tert-butyl cyclohexyl chloroformate craft research. Mainly investigated the reaction time, the reaction temperature, the reactant allocated proportion, the reaction solvent and the catalysts and so on the factor response influences. Summarized the quite good technological conditions: the 4-tert-butyl cyclohexanol dissolves under the room temperature in petroleum ether solution, then slowly adds by drops the BTC petroleum ether solution to the above solution in, and causes it to dissolve completely, then in 60-65℃under heats up the backflow 4 hours coduison responses. Treatment: The majority of solvents will distil off first, (-5℃or so) under resposnse BTC and 4-tert-butyl-cyclohexanol will crystallize in the low temperature, the filtration separation, finally has used th mother liquor the method depuration which the column chromatography. At the same time, had found one fast TLC monitor method in the synthesis, had found a more convenient quick method for the monitoring response. In discussed the BTC and 4-tert-butylb cyclohexanol reaction mechanism, proposed with emphasis the zeolite catalyst reaction mechanism and 4-tert-butyl cyclohexanol and the BTC reaction mechanism, has established 4- uncle the butyl cyclohexanol itself autocatalysis response basis.In the laboratory small trial foundation, we to tested have conducted the pilot test - - experimental enlargement research. In the consideration raw material characteristic and in the technological requirement foundation, we designed a set to suit in the industrialization installment, and has done the optimized experiment, has solved a series of problems which the enlargement experiment appeared, for realized its industrialization to make the preliminary discussion.