- New Pd-phosphorus ylide complexes based on FC60 as heterogeneous nano-catalyst for H/D exchange reaction
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In this account, new Pd(0) complexes of phosphorus ylides based on fullerene C60 (FC60) were synthesized and utilized as the first fullerene-based heterogeneous nano-catalysts for H/D exchange reaction. Four new palladacyclopropa-[60]fullerene complexes 1–4, [(η2-C60)Pd(Y1–4)2] (Y1 = PPh3CHC(O)C6H4-p-NO2, Y2 = PPh3CHC(O)C6H4-p-CH3, Y3 = (p-tolyl)3P-CHC(O)C6H4-p-NO2, and Y4 = (p-tolyl)3P-CHC(O)C6H4-p-CH3), were prepared through dissolving the related α-keto stabilized phosphorus ylide in toluene solution in the presence of FC60 and Pd (dba)2 (dba = dibenzylideneacetone). All of the complexes were characterized using Nuclear magnetic resonance (NMR) (1H, 13C, and 31P), Infrared spectroscopy (IR), Ultraviolet-visible spectroscopy (UV-visible), fluorescence, Electrospray Ionisation Mass Spectrometry (ESI-MS), and Energy-dispersive X-ray spectroscopy (EDX) spectroscopies, and scanning electron microscopy (SEM) and TEM techniques. The data proved that FC60 and two ylides were coordinated to Pd(0) center through two hexagons and two ylidic carbon atoms, respectively. An evaluation was also performed to compare the catalytic activity of synthesized Pd complex 1 and a conventional heterogeneous catalyst, 10% Pd on carbon, in H/D exchange reaction. The results indicate that the process of H/D exchange reaction in aromatic rings of benzoic acid derivatives progressed more efficiently by Pd complex 1.
- Yousefi, Abed,Sabounchei, Seyyed Javad,Hashemi, Ali
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- Deuterium-substituted magnetic resonance dispersion weighted imaging contrast agent
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The invention discloses a deuterium-substituted magnetic resonance dispersion weighted imaging contrast agent. The deuterium-substituted magnetic resonance dispersion weighted imaging contrast agent has high detection resolution and sensitivity, can detec
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- Synthetic method for stable isotope labeled chloramphenicol
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The invention relates to a synthetic method for stable isotope labeled chloramphenicol and belongs to the field of organic synthesis. The synthetic method for stable isotope labeled chloramphenicol ischaracterized in that a stable isotope labeled bromobenzene derivative is taken as a raw material, the raw material is subjected to para-position nitration, cyan substitution, cyan hydrolysis and reduction, and is further oxidized into carbonyl, a substitution reaction is performed on carbonyl and an aromatic ring to obtain amine which is condensed into imine, imine further reacts with ethyl diazoacetate under the action of (R)-VAPOL and triphenyl borate to build an ethylene imine structure, ring opening is performed on ethylene imine under an acid condition, and at last, an ester group is reduced to obtain stable isotope labeled chloramphenicol. The synthetic method is simple in step and simple and convenient to operate; and the product is high in chemical purity and isotope abundance and can be used for internal standard substances for veterinary drug residue test in the food safety field and study of the chloramphenicol metabolic mechanism.
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Paragraph 0041-0043
(2018/07/30)
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- Deuterium-Labeled Precursor Feeding Reveals a New pABA-Containing Meroterpenoid from the Mango Pathogen Xanthomonas citri pv. mangiferaeindicae
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A new para-aminobenzoic-acid-containing natural product from the mango pathogenic organism Xanthomonas citri pv. mangiferaeindicae is described. By means of stable isotope precursor feeding combined with nontargeted LC-MS/MS, the generated spectra were cl
- Saleh, Hesham,Petras, Daniel,Mainz, Andi,Kerwat, Dennis,Nalbantsoy, Ayse,Erzurumlu, Yalcin,Süssmuth, Roderich D.
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supporting information
p. 1532 - 1537
(2016/07/06)
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- Synthesis of deuterium-labelled isotopomer of deferasirox
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A d4-labeled isotopomer of deferasirox was synthesized as internal standard for use in a LC/mass spectroscopy (MS)/MS method developed for the simultaneous quantitative determination of deferasirox in human serum. d4-deferasirox was synthesized from d8-toluene.
- Havaldar, Freddy H.,Dabholkar, Bhushan Vasant,Mule, Ganesh Baban,Kulkarni, Suhas
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p. 163 - 165
(2015/04/27)
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- Synthesis, characterization and applicability of three isotope labeled azobenzene photoswitches
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We describe a short, efficient approach for the synthesis of three novel isotope labeled azobenzene photoswitches. The synthesis is based on commercially available fully isotope labeled precursors. The target molecules have been obtained in good yields, c
- Pfister, Rolf,Ihalainen, Janne,Hamm, Peter,Kolano, Christoph
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experimental part
p. 3508 - 3517
(2009/02/05)
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- Preparation of [2',3',5',6'-2H4]pteroylglutamic acid
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Folic acid plays a key role in nucleic acid biosynthesis, essential for normal cell proliferation and function. Localized folate deficiencies may be related to changes in cytology associated with cancer development; analogs of folic acid, such as methotrexate, are potent chemotherapeutic agents and are widely used either alone or in combination therapy for many types of cancer. In this report we describe the synthesis of a tetra-deuterated folic acid from perdeuterated toluene. The primary intermediate, N-(4-amino [2,3,5,6-2H4]benzoyl)-L-glutamic acid diethyl ester was coupled to N(2')-acetyl-6-formylpterin to create [2',3',5',6'-2H4]folic acid. A similar scheme can be used for the preparation of F [1',2',3',4',5',6'-13C6]folic acid from [13C6] ring labeled toluene.
- Dueker,Jones,Smith,Clifford
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p. 981 - 991
(2007/10/02)
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