- Preparation method of 1-pyrene butyric acid
-
The invention provides a preparation method of 1-pyrene butyric acid, which comprises the following steps: step S1, pyrene and a chloroformyl butyrate compound are subjected to F-C acylation reaction to obtain an intermediate 4-oxo-4-pyrene butyrate; step S2, the intermediate 4-oxo-4-pyrene butyrate and hydrazine hydrate are subjected to Huang Min-long reduction and ester hydrolysis reaction, so as to obtain the 1-pyrene butyric acid. According to the preparation method of the 1-pyrene butyric acid provided by the embodiment of the invention, the chloroformyl butyrate compound is used for replacing succinic anhydride in the prior art for F-C acylation to generate the intermediate 4-oxo-4-pyrene butyrate, and the intermediate 4-oxo-4-pyrene butyrate can be purified by recrystallization of ethanol or methanol, the tedious operation of repeatedly washing with acid and alkali for many times in the process of carrying out F-C acylation reaction by using succinic anhydride is avoided, and the purification difficulty of the product is greatly reduced.
- -
-
-
- Mechanochemical Friedel-crafts acylations
-
Friedel-Crafts (FC) acylation reactions were exploited in the preparation of ketone-functionalized aromatics. Environmentally more friendly, solvent-free mechanochemical reaction conditions of this industrially important reaction were developed. Reaction parameters such as FC catalyst, time, ratio of reagents and milling support were studied to establish the optimal reaction conditions. The scope of the reaction was explored by employment of different aromatic hydrocarbons in conjunction with anhydrides and acylation reagents. It was shown that certain FC-reactive aromatics could be effectively functionalized by FC acylations carried out under ball-milling conditions without the presence of a solvent. The reaction mechanism was studied by in situ Raman and ex situ IR spectroscopy.
- Dud, Mateja,Bri?, Anamarija,Ju?inski, Iva,Gracin, Davor,Margeti?, Davor
-
supporting information
p. 1313 - 1320
(2019/07/08)
-
- Chromophore quench-Labeling: An approach to quantifying catalyst speciation as demonstrated for (EBI)ZrMe2/ b(C6F5)3?Catalyzed polymerization of 1?Hexene
-
Chromophore-containing quench agents 2 and 3 enable quantitative active site counting and determination of the mass distribution of active catalyst polymeryls by refractive index (RI) and UV detected gel permeation chromatography (GPC) for the polymerization of 1-hexene catalyzed by (EBI)ZrMe2/B(C6F5)3. Time evolution of catalyst speciation data and the time profiles of monomer consumption, end-group generation, and bulk molecular weight distribution data have been analyzed by kinetic modeling to determine rate constants for initiation by insertion of hexene into a Zr?Me bond (ki), propagation (kp), chain transfer to form vinylidene (k1,2) and vinylene (k2,1) end groups, and reinitiation from a Zr?H bond (kr). Unlike previous models that assumed fast catalyst reinitiation, this analysis reveals that kr is considerably slower than kp; catalyst speciation data are critical to making this distinction. This study demonstrates that chromophore quench-labeling with 2 and 3 enables rapid, quantitative analysis of detailed kinetic models for catalytic olefin polymerization reactions using GPC with UV and RI detectors.
- Nelsen, D. Luke,Anding, Bernie J.,Sawicki, Julie L.,Christianson, Matthew D.,Arriola, Daniel J.,Landis, Clark R.
-
p. 7398 - 7408
(2018/05/23)
-
- Singly and doubly labeled base-discriminating fluorescent oligonucleotide probes containing oxo-pyrene chromophore
-
We have developed new oxo-pyrene labeled fluorescent nucleoside, Oxo-PyU which showed a strong fluorescence dependency on solvent polarity at long wavelength. The designed singly and doubly Oxo-PyU labeled fluorescent oligonucleotide probes were found highly efficient for the discrimination of A and consecutive AA bases of target DNA opposite to the labeled base via generation of enhanced fluorescence signal.
- Bag, Subhendu Sekhar,Kundu, Rajen,Matsumoto, Katsuhiko,Saito, Yoshio,Saito, Isao
-
body text
p. 3227 - 3230
(2010/10/02)
-
- Pyrene derived functionalized low molecular weight organic gelators and gels
-
Pyrene derived binary functionalized low molecular weight organic gelators (FLMOGs) and gels thereof in selected organic solvents were synthesized and characterized. The functionality refers to a functional group that does not take part in formation of the supramolecular gel network, but remains free and available for other purposes, such as to bind nanoparticles or other molecules into the gel structure. Functional groups were observed to disturb gel formation strongly, if they interact with each other within the same supramolecule due to the formation of competitive structures. Preventing such interactions restored the original gel properties. A gel with weaker supramolecular bonding than the binding between the functional groups was successfully made by separating the functional groups by distance. The π-π-interaction was found to be of negligible significance to the supramolecular binding energy, but probably essential to align the molecules to a one-dimensional chain and bring them into the range of van der Waals forces mainly responsible for the binding in this system. Solvent was observed to increase the binding energy of the supramolecule. All molecules were characterized by spectroscopic techniques and elemental analysis. Selected gels were characterized with rheometry, scanning electron microscopy, UV- and fluorescence spectroscopy. Gelation kinetics and hysteresis were measured by UV-spectroscopy and a fast gelation process was observed for all the gelators studied. The melting enthalpies were measured by DSC and calculated theoretically by PM3 level of theory. The Royal Society of Chemistry and the Centre National de la Recherche Scientifique.
- Hahma, Arno,Bhat, Shreedhar,Leivo, Kimmo,Linnanto, Juha,Lahtinen, Manu,Rissanen, Kari
-
supporting information; body text
p. 1438 - 1448
(2009/02/04)
-
- Compounds for determining the activity of phospholipase A2
-
Compounds for determining the activity of phospholipase A2, are described herein, and include embodiments having formula (1) wherein L1 is derived from an ether (R1—OR2)m, wherein R1 and R2 are independently selected and are derived from a hydrocarbon having 1 to 12 carbon atoms, with m being an integer from 1 to 4, or from a hydrocarbon R having 1 to 20 carbon atoms; F is unsubstituted or substituted pyrene as a flouraphore; Q is a quencher, and L2 is C(O)-L1 or C(O)-L1-NH, wherein L1 is as defined above. These compounds may be used to determine the activity of phospholipase A2, in particular PAF-AH.
- -
-
Page/Page column 7
(2010/11/29)
-