All reagents and chemicals were purchased from commercial sources, including 2,5-dimethyl-2,4-dihydro-3H-pyrazol-3-one (2o ). 1H and 13C nuclear magnetic resonance (NMR) spectra were recorded using a Bruker Avance-400 spectrometer (Bruker BioSpin AG, Fällanden, Switzerland). Deuterated chloroform (CDCl3) and deuterated dimethyl sulfoxide (DMSO-d6) were used as NMR solvents and tetramethylsilane (TMS) was used as an internal standard. Melting points (mp) were recorded on the Hanon MP100 melting point apparatus (Hanon Instruments, Jinan, China). High-resolution mass spectral analysis was carried out using a Varian 7.0 T FTICR-MS instrument (Varian IonSpec, Lake Forest, CA, United States). Single-crystal X-ray data were obtained using a Bruker SMART APEX II X-ray single-crystal diffractometer (Bruker AXS, Karlsruhe, Germany), graphite monochromated Mo Kα radiation (λ = 0.71073 Å), a 3WP-2000-Spray tower (Nanjing Institute of Agricultural Mechanization, Ministry of Agriculture and Rural Affairs, Nanjing, China), and a A560-UV-VIS spectrophotometer (Aoyi Instruments Co., Ltd., Shanghai, China).
Smart apex 2 x ray single crystal diffractometer
Manufactured by Bruker
Sourced in Germany
The SMART APEX II X-ray single-crystal diffractometer is a laboratory instrument designed for the analysis of crystalline materials. It utilizes X-ray technology to collect structural data from single-crystal samples. The core function of the SMART APEX II is to provide precise measurements and analysis of the internal structure and composition of crystalline substances.
Automatically generated - may contain errors
Lab products found in correlation
Uv 3101pc spectrophotometer, by Shimadzu (2 mentions)
7.0 t fticr ms instrument, by Agilent Technologies (1 mentions)
Avance 400 spectrometer, by Bruker (1 mentions)
Avance500 spectrometer, by Agilent Technologies (1 mentions)
Te 2000u fluorescence microscopy, by Nikon (1 mentions)
F 7000 fluorescence spectrophotometer, by Hitachi (1 mentions)
Avance spectrometer, by Bruker (1 mentions)
Jms 600h mass spectrometer, by JEOL (1 mentions)
Vector 22 ftir, by Bruker (1 mentions)
Buchi m 560, by Büchi (1 mentions)
Sabouraud dextrose agar, by Merck Group (1 mentions)
Silica gel, by Merck Group (1 mentions)
Shelxtl 97, by Bruker (1 mentions)
Avance 3 hd 600 spectrometer, by Bruker (1 mentions)
J 1500 circular dichroism spectrophotometer, by Jasco (1 mentions)
6 protocols using smart apex 2 x ray single crystal diffractometer
1
Synthesis and Characterization of 2,5-Dimethyl-2,4-Dihydro-3H-Pyrazol-3-One
2
Synthetic Procedure for PB1-PB4 Pyrrole Dyes
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
A general synthetic
procedure for PB1–PB4 is shown inScheme 1 . The starting reagents were commercially
purchased and used as received without further notice, including 2′,7′-dichlorofluorescin
diacetate (DCFH-DA), 3-ethyl-2,4-dimethyl-1H-pyrrole,
2,3-dimethyl-1H-pyrrole, 4-ethyl-3,5-dimethyl-1H-pyrrole-2-carbaldehyde, 2,2′-(propane-2,2-diyl)bis(1H-pyrrole), trifluoroacetic acid (TFA), 2,3-dichloro-5,6-dicyano-1,4-benzoquinone
(DDQ), N,N-diisopropylethylamine
(NND), 1,3-diphenylisobenzofuran (DPBF), BF3·Et2O, HBr·H2O (48%), POCl3, FeCl3, and NEt3. Organic solvents, such as CH2Cl2 and N,N-dimethylformamide
(DMF), were purified before usage with standard procedures. Compounds
were characterized on a Bruker Avance 300 spectrometer (NMR), an Agilent
1100 MS spectrometer (MS), and a Bruker SMART APEX II X-ray single-crystal
diffractometer (single-crystal XRD). The absorption and emission spectra
were determined using a Hitachi F-7000 fluorescence spectrophotometer
and a Shimadzu UV-3101PC spectrophotometer. Laser power and spectra
were recorded using an Ocean Optics Maya2000 Pro Fiber Optic spectrometer
(excitation = Nd:YAG laser, 10 Hz, 10 ns) and Newport 2936C laser
power meters.
procedure for PB1–PB4 is shown in
purchased and used as received without further notice, including 2′,7′-dichlorofluorescin
diacetate (DCFH-DA), 3-ethyl-2,4-dimethyl-1H-pyrrole,
2,3-dimethyl-1H-pyrrole, 4-ethyl-3,5-dimethyl-1H-pyrrole-2-carbaldehyde, 2,2′-(propane-2,2-diyl)bis(1H-pyrrole), trifluoroacetic acid (TFA), 2,3-dichloro-5,6-dicyano-1,4-benzoquinone
(DDQ), N,N-diisopropylethylamine
(NND), 1,3-diphenylisobenzofuran (DPBF), BF3·Et2O, HBr·H2O (48%), POCl3, FeCl3, and NEt3. Organic solvents, such as CH2Cl2 and N,N-dimethylformamide
(DMF), were purified before usage with standard procedures. Compounds
were characterized on a Bruker Avance 300 spectrometer (NMR), an Agilent
1100 MS spectrometer (MS), and a Bruker SMART APEX II X-ray single-crystal
diffractometer (single-crystal XRD). The absorption and emission spectra
were determined using a Hitachi F-7000 fluorescence spectrophotometer
and a Shimadzu UV-3101PC spectrophotometer. Laser power and spectra
were recorded using an Ocean Optics Maya2000 Pro Fiber Optic spectrometer
(excitation = Nd:YAG laser, 10 Hz, 10 ns) and Newport 2936C laser
power meters.
3
Synthesis of Iridium(III) Complexes
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
The synthetic route for the desired Ir complexes, Ir(ppy)2(BPE) and Ir(ppy)2(TPP), is shown in Scheme 1 . The chemicals and regents involved in Scheme 1 were commercially obtained and used as received, including bis(2-(diphenylphosphanyl)phenyl) ether (BPE), triphenylphosphane (TPP), 2-phenyl pyridine (ppy), KPF6, PVP (K30) and IrCl3·3H2O. MS and NMR spectra were recorded using a Bruker Avance 500 spectrometer and an Agilent 1100 MS spectrometer, respectively. Single crystal diffraction data were obtained with a Bruker SMART APEX II X-ray single crystal diffractometer. Density functional theory calculation was finished with GAMESS at the RB3LYP/LANL2DZ level. A single crystal structure was applied as the initial geometry. Absorption spectra were recorded using a Shimadzu UV-3101PC spectrophotometer. Emission spectra, lifetime, and quantum yield were determined using a Hitachi F-7000 fluorescence spectrophotometer equipped as an integrating sphere. Micromorphology was investigated using a Hitachi S-4800 microscope and a Nikon TE2000-U fluorescence microscopy.
4
Characterization of Mestanolone and Derivatives
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
Mestanolone (1) was acquired from Hangzhu Dayangchem (Cat no. 541-11-9, China). Sabouraud dextrose agar (SDA) was purchased from Merck KGaA (Cat no. 146392, Germany). Silica gel precoated TLC plates (PF254, Merck KGaA, Germany) were used for thin layer chromatography; phosphomolybdic acid solution was used as a staining reagent for UV inactive compounds. Silica gel (70–230 mesh, Merck, Germany) was used for column chromatography. Final purification of the compounds was carried out by using recycling preparative HPLC-LC-908 (Japan), equipped with JAIGEL-ODS-L-80 column, with MeOH–H2O as the mobile phase. Melting points were recorded on Buchi M-560 (Buchi, Switzerland) apparatus. Optical rotations were measured on JASCO P-2000 (JASCO, Japan) polarimeter. UV Spectra were recorded on Hitachi U-3200 (Hitachi, Tokyo, Japan) spectrophotometer. IR Spectra were recorded as KBr discs on Bruker Vector 22 FT-IR (Bruker) spectrometer. Electron ionization (EI-MS) and high resolution electron ionization mass spectra (HREI-MS) were recorded on JEOL JMS600H mass spectrometer (JEOL, Japan). 1H-, 13C- and 2D-NMR spectra were recorded on Bruker Avance spectrometers (Bruker, Switzerland) in CD3OD. X-Ray diffraction data of the compound 6 was recorded on Bruker SMART APEX II single-crystal X-ray diffractometer (Germany).
5
Single Crystal X-ray Structural Analysis
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
X-ray analyses have been performed on Bruker SMART APEX II Single Crystal X-ray Diffractometer equipped with graphite-monochromated Mo-Kα radiation (λ = 0.71073 Å). The crystal structure was solved by direct methods and refined on F2 by full matrix least-squares using Bruker's SHELXTL-97.105 Crystallographic data for the structural analysis have been deposited to the Cambridge Crystallographic Data Center (CCDC 1998538 for 2, CCDC 1998557 for 3, CCDC 1998539 for 7, CCDC 1998546 for 14 and CCDC 1998547 for 20).
6
Comprehensive Analytical Characterization
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
Circular dichroism and optical rotations were measured with JASCO J-1500 circular dichroism spectrophotometer (JASCO, Easton, PA, USA). 1H NMR, 13C NMR and 2D NMR spectra were recorded on a Bruker AVANCE III HD600 spectrometer (Bruker, Billerica, MA, USA) with TMS as reference. The suitable crystal was analyzed on a Bruker Smart Apex II single crystal X-Ray diffractometer (Bruker, Billerica, MA, USA). High-resolution TOFESIMS was performed on a WATERS Xevo G2-S Qtof Quadrupole Time-of-Flight Mass Spectrometry (Waters, Milford, MA, USA). Analysis and semi-preparative reversed-phase HPLC was performed on a Shimadzu LC-2030 liquid chromatography (Shimadzu, Kyoto, Japan) with YMC-Pack ODS-A column 250 × 10 mm i.d., S-5 μm × 12 nm, and 250 × 20 mm i.d., S-5 μm × 12 nm. Column chromatography (CC) was performed on silica gel (200–300 mesh, Jiangyou Silica Gel Co., Ltd., Yantai, China) or CHROMATOREX C18 silica (Fuji Silysia Chemical Ltd., Kozoji-cho, Kasugai Aichi, Japan).
About PubCompare
Our mission is to provide scientists with the largest repository of trustworthy protocols and intelligent analytical tools, thereby offering them extensive information to design robust protocols aimed at minimizing the risk of failures.
We believe that the most crucial aspect is to grant scientists access to a wide range of reliable sources and new useful tools that surpass human capabilities.
However, we trust in allowing scientists to determine how to construct their own protocols based on this information, as they are the experts in their field.
Ready to get started?
Sign up for free.
Registration takes 20 seconds.
Available from any computer
No download required
Revolutionizing how scientists
search and build protocols!