20062-22-0Relevant articles and documents
A Green and Effective Approach of Two-Step 2,2′,4,4′,6,6′-Hexanitrostilbene Preparation and Its Industrial Scale Study
Wang, Pengcheng,Lu, Ting-Ting,Lu, Ming
, p. 668 - 674 (2016)
An environmental friendly approach for two-step synthesis of hexanitrostilbene (HNS) has been studied here. In the first step from trinitrotoluene (TNT) to hexanitrobienzyl (HNBB), commercial NaClO was employed as oxidant in mixed solvent of ethyl acetate/ethanol (0.25 mL/1.25 mL per mmol of TNT) instead of benzene/ethanol. In the second step from HNBB to HNS, 2,2,6,6-tetramethylpiperidine-1-oxyl (TEMPO)/FeCl2 was used as an effective catalytic system with O2 in DMSO solvent. A complex of metal ion and O2 [M(n+1)OO?] was supposed to be the active agent, and TEMPO itself was difficult to initiate dehydrogenation of HNBB but could promote the catalytic cycle of complex M(n+1)OO?. Finally, we increased the scale from 30 to 1000 g to investigate the feasibility of production. The total yield of two steps would be unprecedentedly as high as 70%.
Preparation method and application of O-nitrobenzaldehyde
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Paragraph 0050-0052, (2020/09/23)
The invention relates to a preparation method of o-nitrobenzaldehyde. The preparation method comprises the following steps: reacting o-nitrobenzyl triphenylphosphonium bromide with the required product o-nitrobenzaldehyde as raw materials to generate 1, 2-bis (o-nitrophenyl) ethylene, and oxidizing with ozone to obtain o-nitrobenzaldehyde. The preparation method has the beneficial effects that only a proper amount of alkali is used for catalysis in a condensation reaction, and an intermediate product 1, 2-bis (o-nitrophenyl) ethylene can be efficiently obtained by catalysis of an alkaline water reaction; and gas-liquid reaction is performed by using a micro-channel reactor to finally obtain the required nitrobenzaldehyde. The method has the advantages of less used raw materials, high reaction yield, less by-products and impurities, simple and feasible purification operation, and convenience for industrial production in workshops. Under the condition that the current chemical engineering environment protection and safety situation is severe, the process route can stably supply the important chemical intermediates of the type in an environment-friendly mode with the extremely high atom utilization rate.
Synthetic method of hexanitrostilbene
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Paragraph 0019-0020; 0025-0030, (2017/09/01)
The invention discloses a synthetic method of hexanitrostilbene (HNS). The method is used for solving the problems of high quality requirement, difficult weighing and irritant gas generation of liquid bromine used in the process for synthesizing the HNS from hexanitrobibenzyl. The HNS is prepared from the hexanitrobibenzyl under the action of a solid dehydrogenating agent by using a mixed solvent as a solvent. The method is mainly used for synthesizing the HNS.