Chemicals were purchased from commercial suppliers and were used without further purification unless otherwise noted. For thin layer chromatography (TLC) aluminium backed silica gel 60 F254 (from Merck) was used. Flash column chromatography was performed with a Büchi Sepacore MPLC system using silica gel 60 M (particle size 40–63 μm) or conventional glass columns. Preparative TLC was performed on glass backed silica gel GF uniplates (1000 microns) from Analtech. Melting points were measured on a Büchi B-545 melting point apparatus and are uncorrected. 1H NMR and 13C NMR spectra were recorded from CDCl3 solutions on a Bruker AC 200 (200 MHz), a Bruker Avance UltraShield 400 (400 MHz) or a Bruker Avance III HD 600 (600 MHz) spectrometer. Chemical shifts are reported in ppm relative to the nominal residual solvent signals of CDCl3: 1H NMR: 7.26 ppm, 13C NMR: 77.16 ppm. HRMS data was measured with a Shimadzu HPLC-IT-TOF mass spectrometer (ESI).
B 545 melting point apparatus
Manufactured by Büchi
Sourced in Switzerland
The B-545 melting point apparatus is a laboratory instrument designed to determine the melting point of solid samples. It features a heating block, temperature control, and a digital display to precisely measure the melting temperature of a sample.
Automatically generated - may contain errors
Lab products found in correlation
Ac 200, by Bruker (2 mentions)
Avance ultrashield 400, by Bruker (2 mentions)
Avance 3 hd 600, by Bruker (1 mentions)
Amx400, by Agilent Technologies (1 mentions)
Unity plusvarian 500, by Agilent Technologies (1 mentions)
Silica p flash silica gel, by Silicycle (1 mentions)
Perkin elmer 2400 chn analyzer, by PerkinElmer (1 mentions)
Merck kieselgel 60 f254, by Merck Group (1 mentions)
Mat incos 50, by Thermo Fisher Scientific (1 mentions)
Avance 600 spectrometer, by Bruker (1 mentions)
Avance 500 spectrometer, by Bruker (1 mentions)
Autopurification system, by Waters Corporation (1 mentions)
6230 lc tofms mass spectrometer, by Agilent Technologies (1 mentions)
Dual ajs esi source, by Agilent Technologies (1 mentions)
Silica gel 60 f254 plate, by Merck Group (1 mentions)
Mpf 4 spectrofluorimeter, by Hitachi (1 mentions)
Ftir 8400, by Shimadzu (1 mentions)
J 1500 cd spectrometer, by Jasco (1 mentions)
6 protocols using b 545 melting point apparatus
1
Organic Compound Characterization Protocol
2
Purification and Characterization of Organic Compounds
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
Column chromatography was performed on silica gel (Silica-P flash silica gel from Silicycle, size 40–63 μm). TLC was performed on silica gel 60/Kieselguhr F254. Mass spectra were recorded on an AEI-MS-902 mass spectrometer (EI+) or a LTQ Orbitrap XL (ESI+). 1H, 13C, and 19F NMR were recorded on a Varian AMX400 (400, 100.6, and 376 MHz, respectively) or a Varian Unity Plus Varian-500 (500, 125, and 471 MHz, respectively). Chemical shift values for 1H and 13C NMR are reported in ppm with the solvent resonance as the internal standard (CHCl3: δ 7.26 ppm for 1H, δ77.0 ppm for 13C). Data are reported as follows: chemical shifts, multiplicity (s = singlet, d = doublet, t = triplet, q = quartet, br = broad, m = multiplet), coupling constants (Hz), and integration. Melting points were determined on a Buchi B–545 melting point apparatus. All reactions were performed under anhydrous conditions and under N2 atmosphere. All chemicals used were of analytical grade and were used as received without any further purification. All anhydrous solvents used in reactions were purchased in SureSeal bottles or dried over molecular sieves. Flash column chromatography was performed on Biotage Isolelera One with prepacked columns.
3
Synthesis and Characterization of Pyrazole Derivatives
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
Melting points were measured in open capillary tubes on a BÜCHI B-545 melting point apparatus (BÜCHI Labortechnik AG, Flawil, Switzerland) and were uncorrected. Elemental analyses (C, H, N) were performed using the Perkin-Elmer 2400 CHN analyzer (PerkinElmer, Waltham, MA, USA), with results within ±0.4% of the theoretical values. The 500 MHz 1H and 100 MHz 13C NMR spectra were recorded on a Varian Unity Plus 500 (500 MHz) spectrometer (Varian Inc., Paulo Alto, CA, USA). All spectra were recorded at room temperature, unless specified otherwise, and were referenced internally to solvent reference frequencies. Chemical shifts (δ) are presented in ppm and coupling constants (J) in Hz. LC-MS spectra were obtained on a Finnigan MAT INCOS-50 (Thermo Finnigan LLC, San Jose, CA, USA). The reaction mixture was monitored by thin-layer chromatography (TLC) using commercial glass-backed TLC plates (Merck Kieselgel 60 F254, Merck, Darmstadt, Germany). Solvents and reagents that are commercially available were used without further purification. The synthesis of 1,3-diphenyl-1H-pyrazole-4-carbaldehyde (i) and thiazolidine-2,4-dione (ii) was carried out according to methods described in references [53 (link),54 ], respectively.
4
Characterization of Organic Compounds
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
Melting points were measured in open capillary tubes on a BÜCHI B-545 melting point apparatus (BÜCHI Labortechnik AG, Flawil, Switzerland) and are uncorrected. The elemental analyses (C, H, N) were performed using the Perkin–Elmer 2400 CHN analyzer (PerkinElmer, Waltham, MA, USA) and were within ±0.4% of the theoretical values. The 500 MHz-1H and 126 MHz-13C spectra were recorded on Bruker AVANCE-500 spectrometer and 2D spectra were recorded on a Bruker AVANCE-600 spectrometer (Bruker, Bremen, Germany). All spectra were recorded at room temperature except where indicated otherwise and were referenced internally to solvent reference frequencies. Chemical shifts (δ) are quoted in ppm and coupling constants (J) are reported in Hz. LC-MS spectra were obtained on a Finnigan MAT INCOS-50 (Thermo Finnigan LLC, San Jose, CA, USA). Solvents and reagents that are commercially available were used without further purification. The synthetic procedure for compound 1 was described in [48 (link)], for derivatives 2 a–l in [29 (link)] and for compound 4 in [35 (link)].
5
Synthesis and Characterization of Heterocyclic Compounds
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
Commercially available reagents were used without further purification. Reactions were monitored by thin layer chromatography with silica gel 60 F254 plates (E. Merck, Darmstadt, Germany). HPLC chromatography was carried out with the Autopurification system by Waters using fluoro-phenyl columns. 1H and 13C NMR spectra were recorded on Bruker AC 200 (1H: 200 MHz, 13C: 50 MHz), Bruker Avance Ultrashield 400 (1H: 400 MHz, 13C: 101 MHz) or Bruker Avance IIIHD 600 spectrometer equipped with a Prodigy BBO cryo probe (1H: 600 MHz, 13C: 151 MHz). Chemical shifts are reported in parts per million (ppm) and were calibrated using DMSO-d6 as internal standard. Multiplicities are denoted by s (singlet), br s (broad singlet), d (doublet), dd (doublet of doublet) and m (multiplet). Melting points were determined with a Büchi Melting Point B-545 apparatus. HR-MS was measured on an Aglient 6230 LC TOFMS mass spectrometer equipped with an Aglient Dual AJS ESI-Source.
Compounds1 (PZ II 028), 2 (LAU156), 3 (LAU206) and 4 (LAU176) were synthesized and published previously23 (link). Synthesis of 5 (DCBS76) was conducted in analogy to previously outlined synthetic routes23 (link), 44 (link), 45 (link). The synthesis of 6 (DCBS96) was improved as described. Compound 7 (LAU462) was synthesized according to reported protocols23 (link), 46 (link), 47 (link).
Compounds
6
Synthesis and Characterization of Chiral Amines
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
Propylamine,
butylamine, sec-butylamine (α-chiral amine), tert-butylamine, pentylamine, isopentylamine, tert-pentylamine, hexylamine, 2-aminoheptylamine (α-chiral amine),
octylamine, chloroacetic acid, glycine, and hydrochloric acid were
purchased from Sigma-Aldrich and Merck. Acetone and n-octanol were of analytical grade and used as received. IR spectra
were collected on an FT-IR 8400 Shimadzu spectrometer using KBr pellets.
The mass spectra were scanned using a model CH7A Varian (EI, 70 eV)
mass spectrometer. 1H NMR (300 MHz) and 13C
NMR (75 MHz) spectra were recorded on a Bruker BRX-250 Avance spectrometer.
Chemical shifts for 1H were referenced to the residual
proton in the DMSO-d6 solvent. Melting
points were measured using a BUCHI melting point B-545 apparatus.
Further, through a SPEKOL 2000 UV 6800 recording spectrophotometer,
the absorbance was measured. A Jasco J-1500 CD spectrometer was employed
to measure the circular dichroism. A Jasco J-1500 CD spectrometer
and a Hitachi MPF-4 spectrofluorimeter were employed to measure the
circular dichroism and the fluorescence emissions, respectively. Viscosity
measurement was studied by an Ostwald microviscometer (Schott-Geräte).
The optical density (OD) was measured spectrophotometrically at 570
nm via a BioTek-ELx800 Eliza microplate reader.
butylamine, sec-butylamine (α-chiral amine), tert-butylamine, pentylamine, isopentylamine, tert-pentylamine, hexylamine, 2-aminoheptylamine (α-chiral amine),
octylamine, chloroacetic acid, glycine, and hydrochloric acid were
purchased from Sigma-Aldrich and Merck. Acetone and n-octanol were of analytical grade and used as received. IR spectra
were collected on an FT-IR 8400 Shimadzu spectrometer using KBr pellets.
The mass spectra were scanned using a model CH7A Varian (EI, 70 eV)
mass spectrometer. 1H NMR (300 MHz) and 13C
NMR (75 MHz) spectra were recorded on a Bruker BRX-250 Avance spectrometer.
Chemical shifts for 1H were referenced to the residual
proton in the DMSO-d6 solvent. Melting
points were measured using a BUCHI melting point B-545 apparatus.
Further, through a SPEKOL 2000 UV 6800 recording spectrophotometer,
the absorbance was measured. A Jasco J-1500 CD spectrometer was employed
to measure the circular dichroism. A Jasco J-1500 CD spectrometer
and a Hitachi MPF-4 spectrofluorimeter were employed to measure the
circular dichroism and the fluorescence emissions, respectively. Viscosity
measurement was studied by an Ostwald microviscometer (Schott-Geräte).
The optical density (OD) was measured spectrophotometrically at 570
nm via a BioTek-ELx800 Eliza microplate reader.
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!