Ropic liquid. Both 5b and 5c show a sturdy diffraction peak in the small-angle region (two = 3.8or four.5, a broad halo peak from the alkyl chain at ca. 18 plus a core ore distance peak at three.5.7 ConsideringFigure five: X-ray diffraction profiles of four at distinct temperatures.Beilstein J. Org. Chem. 2013, 9, 2852861.(Figure 2A). The lattice parameters in the discotic Col mesophase with the trimers are summarized in Table 2. Trimer four displayed a smaller intracolumnar core ore distance of 3.57than that of 5b and 5c, because of the stronger interactions between the triphenylene discogens with mono-ester group. The columnar parameter values with the trimers decreased using the spacer length shortened. So we deduced that the benzene cores had been among the alkyl chains inside the columnar stacking of the trimers.ranges which includes space temperature. The connecting linker group towards the triphenylene and the spacer length for the central benzene core have crucial impacts around the supramolecular packing and phase-transition temperature. We anticipate that this Co2(CO)8-catalyzed synthetic strategy may be applied for the synthesis of liquid crystalline polymer networks.ExperimentalInstruments and situations: See Supporting Details File 1.Table 2: Columnar mesophase parameters on the DLC trimers.Chemical reagents and starting materials10-undecynoic acid, 5-chloro-1-pentyne, propargyl bromide and Co2(CO)eight had been bought from Alfa Aesar (Tianjin, China). All of the other reagents and solvents have been industrial solutions and utilized without having additional purification unless otherwise noted.R-Phycoerythrin 10-Undecyn-1-yl p-toluenesulfonate [53,54], 2-hydroxy3,six,7,ten,11-pentakis(pentyloxy)triphenylene [52] were synthesized as described in the reported procedures.Imatinib Monomer two, C18H6(OC5H11)5(OOCC8H16-CCH): Monomer two was prepared similar towards the reported technique [52]. The mixture of 10-undecynoic acid (218 mg, 1.two mmol), dicyclohexylcarbodiimide (DCC, 247 mg, 1.two mmol), 4-N,N-dimethylaminopyridine (DMAP, 67 mg), and 2-hydroxy-3,6,7,ten,11pentakis(pentyloxy)triphenylene (1, 674 mg, 1.0 mmol) in CH2Cl2 (20 mL) was stirred at space temperature for six h beneath a nitrogen atmosphere. Immediately after the reaction was completed, water was added for the mixture after which extracted with CH2Cl2. The extract was dried with MgSO4 plus the solvent was distilled off making use of a rotary evaporator.PMID:23996047 The crude solution was purified by column chromatography on silica gel eluted with CH 2 Cl two / hexane (three:two in volume). The solution was re-crystallized from ethanol affording a white strong (543 mg, 0.65 mmol, 65 ). 1H NMR (CDCl3, TMS, 400 MHz) eight.06 (s, 1H, ArH), 7.85.77 (m, 5H, ArH), 4.26.19 (m, 10H, CH2), 2.67 (t, J = 7.six Hz, 2H, CH2), 2.20 (td, J = 7.2 Hz, J = two.eight Hz, 2H, CH2), 1.96.87 (m, 13H, CH2, CCH), 1.57.39 (m, 30H, CH2), 0.99.97 (t, J = 7.2 Hz, 15H, CH3). Monomer 3a, C18H6(OC5H11)5(OC9H18-CCH): The mixture of 10-undecyn-1-yl p-toluenesulfonate (387 mg, 1.2 mmol), K 2 CO three (345 mg, 2.5 mmol), and 2-hydroxy-3,six,7,ten,11pentakis(pentyloxy)triphenylene (1, 74 mg, 1.0 mmol) in DMF (15 mL) was stirred at 80 for 24 h below N2. The mixture was cooled to area temperature, and 3 M HCl was added dropwise until the mixture was acidic. The organic phase was extracted with CH2Cl2 and dried over anhydrous MgSO4. The solvent was evaporated under decreased pressure to afford the crude product, which was purified by column chromatography on silica gel eluted with CH 2 Cl two /hexane. The solution was re-crystallized from ethanol to afford a light yellow solidCompd. four (25 )hkl.
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