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Preparation method of TAT

A mass ratio, acetic anhydride technology, applied in the direction of organic chemistry, can solve the problems of lack of application prospects, large consumption of acetic anhydride, large consumption of acetic anhydride and acetyl chloride, etc., to achieve cost reduction, simple process, and constant yield Effect

Inactive Publication Date: 2010-07-07
ZHONGBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Among the above several preparation methods, method 1 consumes too much acetic anhydride and acetyl chloride, if adopt lower temperature (0~10 ℃ or lower), then need the required expensive refrigerating equipment of low temperature operation, if at high temperature Carrying out at room temperature (such as 50°C) greatly accelerates unwanted side reactions at high temperatures and reduces the yield of TAT
And the reaction process is difficult to control; method 2 consumes too much acetic anhydride; method 3 needs to add a solid catalyst and needs to be filtered
The existence of these objective factors makes these methods lack application prospects

Method used

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  • Preparation method of TAT
  • Preparation method of TAT

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 7g (0.05mol) of HA, 3.1g (0.04mol) of ammonium acetate and 3.5g (0.2mol) of water into a round-bottomed flask, stir to form a slurry, control the temperature of the system at 5-10°C, and stir for 30 minutes Slowly add 15 g of acetic anhydride (0.15 mol) dropwise. After the addition, control the temperature below 10°C and continue stirring for 30 min to complete the reaction. The temperature of the reaction solution was raised to 120° C. and distilled under reduced pressure. 20 mL of acetone was added to the obtained product and heated to boil for recrystallization to obtain 10.6 g of white crystals of DAPT with a yield of 100% (based on the added HA).

[0021] Add 5g (0.024mol) of DAPT and 9.6g (0.09mol) of acetic anhydride into the reactor, heat up to 110C for 2h under stirring, cool down to 30°C, add 2mL of water for 1.5h, distill under reduced pressure, and dilute the obtained The yellow solid product was recrystallized with boiling acetone to obtain 5.48 g of th...

Embodiment 2

[0031] Add 9.5g (0.068mol) of HA, 5g (0.065mol) of ammonium acetate and 6mL (0.343mol) of water (water temperature 5-10°C) into a 50mL round bottom flask, stir to form a slurry, and control the temperature of the system at 5-10°C. ℃, slowly add 18g of acetic anhydride (0.18mol) dropwise within 50min under stirring, after the addition, control the temperature below 10℃, and continue stirring for 40min to complete the reaction. The reaction solution was heated to 120°C for distillation under reduced pressure, 40 mL of acetone was added to the distilled product, and after heating and boiling, recrystallization was carried out to obtain 14.38 g of white crystals of DAPA, with a yield of 100% (based on the added HA).

[0032] Add 8gDAPT and 16.7g acetic anhydride into a 100mL reactor, raise the temperature to 100°C for 2h under stirring, cool down to 30°C, add 4mL of water to react for 1.5h, distill under reduced pressure, and recrystallize the obtained pale yellow solid product wit...

Embodiment 3

[0034] Add 22g (0.157mol) of HA, 9.5g (0.123mol) of ammonium acetate and 11mL (0.628mol) of water (water temperature 5-10°C) into a 50mL round bottom flask, stir to form a slurry, and control the temperature of the system at 5-10°C. ℃, slowly add 50g of acetic anhydride (0.5mol) dropwise within 30min under stirring, after the addition, control the temperature below 10℃, continue stirring for 35min to complete the reaction. The temperature of the reaction solution was raised to 120° C. for distillation under reduced pressure, 30 mL of acetone was added to the product, and recrystallization was carried out after heating and boiling to obtain 33.14 g of white crystals of DAPA, with a yield of 100% (based on the added HA).

[0035] Add 10gDAPT and 19.2g acetic anhydride into a 100mL reactor, raise the temperature to 110°C for 2h under stirring, cool down to 30°C, add 3mL of water to react for 1.5h, distill under reduced pressure, and recrystallize the obtained pale yellow solid produ...

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Abstract

The invention relates to a preparation method of TAT, comprising the following steps of: slowly dripping acetic anhydride with 1.5-2.5 times of the mass of HA at 5-10 DEG C by using the HA, ammonium acetate and water as raw materials; reacting for 30-50 minutes to obtain DAPA under stirring; reacting for 2-3 hours by using DAPT and the acetic anhydride as the raw materials and increasing temperature to 100-110 DEG C; and reacting for 1-2 hours by reducing the temperature to 30-35 DEG C to obtain a product TAT, in the presence of water as a catalyst, wherein the water accounts for 5-35 percent of the mass of the acetic anhydride raw material. The invention replaces the catalyst in a Lukasavage process method with the inexpensive water, obviously enhances the yield of the TAT, enables the synthesizing process of the TAT to be easy and reduces the production cost.

Description

technical field [0001] The invention relates to a preparation method of an energetic material intermediate, in particular to a preparation of 1,3,5,7-tetraacetyl-1,3,5,7-tetraazacyclooctane (TAT) method. Background technique [0002] TAT (1,3,5,7-tetraacetyl-1,3,5,7-tetraazacycloctane) is one of the important intermediates for the synthesis of HMX (Octogen), and can also be used in solution Suspending agent, stabilizer, etc., select a suitable nitrating agent to nitrate TAT, and high yield and high purity HMX can be obtained. Since the 1970s, many scientific research units have begun to study the synthesis method of TAT, improved the original process, and achieved certain results, injecting new vitality into the application of TAT. So far, the preparation of TAT mainly has the following methods: [0003] 1. In 1972, American researchers reacted urotropine, acetic anhydride, water and ammonium acetate at 0-20°C to generate DAPT (1,5-diacetyl-3,7-methano-1 , 3,5,7-tetraaza...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D257/02
Inventor 王建龙陈丽珍曹端林李永祥李全良徐春彦
Owner ZHONGBEI UNIV
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