16968-19-7Relevant articles and documents
Ivanoff,Zidaroff
, p. 420 (1962)
Solvent-Free Synthesis of Diazocine
Moormann, Widukind,Langbehn, Daniel,Herges, Rainer
, p. 3471 - 3475 (2017)
A convenient two-step synthesis of diazocine starting from 2-nitrotoluene is described. The first step, the oxidative dimerization of 2-nitrotoluene, is improved to 95% yield. The second step, the reductive azo cyclization, is performed as a solvent-free reaction with lead powder in a ball mill (51% yield). As a reference, the previously described azo cyclization with Zn/Ba(OH) 2 is investigated in detail. The results explain why in previous experiments the yields are low and extremely dependent on the reaction conditions. In view of potential applications in photopharmacology, we checked the stability under reducing conditions. Diazocine does not react with glutathione, indicating intracellular stability.
Method of preparing 2,2'-binitrobibenzil
-
Paragraph 0020; 0022, (2017/11/16)
The invention discloses a method of preparing 2,2'-binitrobibenzil by a catalysis method and a preparation method of a catalyst used by the preparation method. The preparation method of 2,2'-binitrobibenzil comprises the steps of taking ortho-nitrobenzyl chloride as a raw material and methyl chloride as a solvent, adding an amine sacrifice agent, taking a noble metal gold loaded nano titanium oxide carrier as the catalyst, performing a reaction under light irradiation, performing sufficient ultrasonic dispersion prior to the reaction, performing solvent reflux in a reaction process, stirring a reaction system in the reaction process to keep the reaction system in a suspension state, and performing solid-liquid separation after reaction completion to obtain a coupled product, namely 2,2'-binitrobibenzil. The preparation method greatly reduces energy consumption caused by a high temperature in the traditional technology, and avoids cost increase and product loss caused by multi-step and multi-time purification; three wastes generated in a production process are few; a technology is concise; a yield of a product is higher; and a green chemistry concept is met.
Heterogeneous photocatalytic C-C coupling: Mechanism of plasmon-mediated reductive dimerization of benzyl bromides by supported gold nanoparticles
Lanterna, Anabel E.,Elhage, Ayda,Scaiano, Juan C.
, p. 4336 - 4340 (2015/09/01)
The use of gold nanoparticles supported on TiO2 (Au@TiO2) as photocatalysts was extended to include photoinduced reductive C-C coupling. Surface plasmon excitation of supported AuNPs in the presence of an amine leads to the C-C coupling of a variety of substituted benzyl bromides at room temperature with good yields in a free radical-mediated reaction. The overall efficiency of the C-C coupling is largely dependent on the nature of the amine used.