trichlorotrinitrobenzene

     Trichlorotrinitrobenzene, or more properly 1,3,5-trichloro-2,4,6-trinitrobenzene, is a high explosive material used primarily as a chemical intermediate. While trichlorotrinitrobenzene is an explosive in its own right, it is mostly used to prepare TATB.

CHEMICALS	APPARATUS
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     Synthesis 1: Into a 1000-mL round-bottomed flask containing 310 mL of 100% sulfuric acid slowly add 77 g of sodium nitrate while stirring. The nitrate addition will generate large amounts of heat, so cooling the beaker in an ice bath may be required. Once all of the nitrate has been added and the solution no longer generates its own heat, warm the solution to 100 C. Add in one portion 25 g of 1,3,5-trichlorobenzene and quickly raise the temperature of the solution to 145-155 C. Maintain a temperature around 150 C for 4 hours. A small amount of toxic gas may be released during this time, so have some ventilation handy. Once the reaction time has elapsed allow the contents of the flask to cool to 40 C. Pour the entire contents of the flask into a large beaker containing 1.2 Kg of crushed ice while stirring. A precipitate should form and more fumes may be given off. Drown the mixture with ice water to dilute the acid and decant off as much liquid as possible. Pour the remaining precipitate over a filter to collect it. Wash the crystals of trichlorotrinitrobenzene with several 1 L portions of water until the wash is between pH 6 and 7. This sample can be used, while still wet, in the preparation of TATB synthesis 1. Synthesis 2: Step 1: Into a 400-mL beaker immersed in an ice bath prepare a mixture of 50 mL of 90% nitric acid and 115 mL of 94% sulfuric acid. Slowly add, with stirring, 35.4 g of 3,5-dichloroanisole over a period of 2 minutes. Wait 3 minutes after the addition, and then slowly heat the beaker on a steam bath to 100 C over a period of 8 minutes. Hold at 100 C for 15 minutes before allowing the mixture to cool to room temperature. Pour the mixture into a large beaker containing an excess of ice and stir until most of the ice melts. The precipitated product can be filtered to collect it, washed thoroughly with water until no trace of acid remains, and dried. Final yield of 3,5-dichloro-2,4,6-trinitroanisole is about 62 g or 99%. The 3,5-dichloro-2,4,6-trinitroanisole can be purified by recrystallizing from a mixture of toluene and hexane. Step 2:

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