Sythesis Of 2
The trinitration in the laboratory is conveniently carried out without separating the 2,4-dinitrotoluene from the spent acid.
While the dinitration mixture is stirred actively at a temperature of about 90° C, 145 grams of fuming sulfuric acid (oleum containing 15% free sulfur trioxide) is added slowly by pouring from a beaker.
To the round bottom flask containing calculated amount of nitrating mixture, 40 g of dinitrotoluene are slowly placed.
The reaction mixture is starting gently to heat until the temperature reaches 80° C.
All the product is washed three or four times by agitating it vigorously with hot water under which it is melted.
After the last washing, the TNT is granulated by allowing it to cool slowly under hot water while the stirring is continued.
The spent acid contains considerable TNT in solution; this is precipitated by pouring the acid mixture into a large volume of water, filtered off, rinsed with water, and added to the main batch.At this temperature distilled waters is slowly added to the reaction mixture and the reaction product is separated as a yellow oil in a separation funnel.Then the reaction product is further washed with distilled water, diluted sodium carbonate solution in order to remove the inorganic acids.The addition of the acid will require about 1 hour.After the acid has been added, the mixture is stirred for 2 hours longer at 90-100° C to complete the nitration. The upper layer consists largely of 2,4-dinitrotoluene, but probably contains a certain amount of 2,4,6-trinitrotoluene.If we just barrel along, doing bromination first and nitration second, what happens?Since the first reaction (bromination) installs an you have a list of some of the reactions needed to form/break these bonds, you need to ask a third question when planning a synthesis: “In what order do we run these reactions?In planning a synthesis, the order in which reactions are done can have a crucial impact on the outcome!Say you want to make this compound, This is where “order of operations” rears its potentially ugly head.An efficient ruthenium-catalyzed synthesis of tri-substituted 1,3,5-triazinones from alcohols and guanylureas under mild conditions has been developed.The scope of both the alcohols and guanylureas in the reaction is demonstrated.