27414-57-9Relevant articles and documents
Method for using microchannel reactor to prepare paracyclophane monomeric compound
-
Paragraph 0054; 0058-0061, (2017/08/23)
The invention discloses a method for using a microchannel reactor to prepare a paracyclophane monomeric compound. The method comprises the steps of preheating, intermediate synthesizing, product synthesizing, oil-water separating, purifying and the like. The paracyclophane monomeric compound is prepared in the continuous microchannel reactor. The method for using the microchannel reactor to prepare the paracyclophane monomeric compound has the advantages of being low in cost and small in energy consumption, having less three wastes, having continuous controllability, having no amplification effect and the like, and is capable of being subjected to simple amplification with equal ratio according to a demand of practical production.
A two-chloro to di-methyl benzene ring II method of making
-
Paragraph 0023; 0024; 0025, (2017/08/18)
The invention discloses a preparation method of dichloro-p-xylene cyclic dimer, which comprises the following steps: respectively adding ammonium N-(3-chloro-4-methylbenzyl)-trimethyl-chloride, a solvent and a catalyst into a reactor provided with a condenser, a stirrer and a thermometer, adding an alkali solution into the reactor at 70-115 DEG C to carry out cyclization reaction, and stirring for 6.5-12 hours to obtain a dichloro-p-xylene cyclic dimer crude product; and carrying out vacuum filtration on the obtained crude product, and purifying by recrystallizing with an organic solvent to obtain the target product dichloro-p-xylene cyclic dimer. The preparation method is simple to operate, and has the advantages of favorable selectivity and high target yield; and the trimethylamine generated in the reaction process can be recovered. The whole technique is safe and environment-friendly, has the advantages of low cost and favorable economic benefit, and belongs to a green chemical technique.
4,15-Diamino[2.2]paracyclophane as a starting material for pseudo-geminally substituted [2.2] paracyclophanes
El Shaieb, Kamal,Narayanan, Vijay,Hopf, Henning,Dix, Ina,Fischer, Axel,Jones, Peter G.,Ernst, Ludger,Ibrom, Kerstin
, p. 567 - 577 (2007/10/03)
Diazotization of the title compound 3, followed by treatment of the formed bis(diazonium ion) with cuprous chloride, yields the pseudo-geminal dichloride 1. Similarly, 3 is converted into the bis(azide) 5 when sodium azide is used as the trapping nucleophile. Hypochlorite oxidation of 3 furnishes the azo compound 4, the first multi-bridged cyclophane with a bridge consisting only of heteroatoms. Reduction of 4 with zinc/acetic acid affords the substrate 3 again. Treatment of 4 with bromine/iron powder or iodine monochloride causes deazotization accompanied by halogen introduction in pseudo-geminal position (i.e., formation of 2 and 6, respectively). Flash vacuum pyrolysis (450 °C, 0.01 Torr) of 4 produces the phenanthrene derivatives 13 and 14, while with tetracyanoethylene (TCNE) the azophane undergoes rapid cycloaddition at room temperature to give the [2+4] cycloadduct 16. The structures of 1, 2, 4-6, and 16 have been determined by X-ray structural analysis. Molecular packing patterns are determined by weak hydrogen bonds; a common packing pattern for cyclophane derivatives is ascribed to C-H...π interactions. Full bandshape analyses of the bridge proton signals in the 1H NMR spectra of 1, 2, 6, and of the difluoro analogue 17 yielded the vicinal 1H,1H coupling constants. These reflect the 1:1 equilibrium between the two skew conformations of the bridges. Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2003.
