Melting points were measured using a Boetius hot plate microscope and are uncorrected. 1H NMR and 13C NMR spectra were recorded on a Varian Gemini 300BB operating at 300 MHz for 1H and 75 MHz for 13C. The spectra were recorded in CDCl3 or DMSO-d6 at 298 K and the chemical shifts are relative to TMS used as the internal standard. The bidimensional correlations spectra (COSY, HETCOR) were performed for complete assignment of chemical shifts. Fourier-transform IR spectra (for representative compounds) were recorded on a Bruker Vertex 70 spectrometer with horizontal device for attenuated reflectance and diamond crystal, in a spectral window ranging from 4000 to 400 cm−1 or on a Nicolet Impact 410 Spectrometer in KBr pellets. Elemental analysis was performed on a Perkin Elmer CHNS/O analyzer Series II 2400 apparatus and the results were in agreement with the calculated values. All starting materials and solvents were purchased from common commercial suppliers and were used without purification unless otherwise noted.
Gemini 300bb
Manufactured by Agilent Technologies
Sourced in United States
The Gemini-300BB is a benchtop NMR spectrometer designed for routine analysis and characterization of chemical compounds. It provides high-resolution, high-sensitivity nuclear magnetic resonance (NMR) capabilities for a variety of sample types. The Gemini-300BB features a 300 MHz superconducting magnet and supports multiple nuclei detection.
Automatically generated - may contain errors
Lab products found in correlation
Chns o analyzer series 2 2400 apparatus, by PerkinElmer (1 mentions)
Vertex 70 spectrometer, by Bruker (1 mentions)
Silica gel 60 gf254, by Merck Group (1 mentions)
Mercury 500, by Agilent Technologies (1 mentions)
Ft ir vertex 70 spectrometer, by Bruker (1 mentions)
Avance 3, by Bruker (1 mentions)
Ft ir 8400s spectrophotometer, by Schimadzu (1 mentions)
Ft ir 4200 spectrometer, by Jasco (1 mentions)
2400 series 2 chns o elemental analyzer, by PerkinElmer (1 mentions)
5 protocols using gemini 300bb
1
Characterization of Organic Compounds
2
Synthesis and Characterization of Novel Compounds
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All starting materials were purchased from Sigma-Aldrich (Germany). Melting points (°C) were determined with a Gallenkamp melting point apparatus (London, UK), and are uncorrected. 1HNMR and 13CNMR were performed in NMR department, Faculty of Science, Mansoura University, Mansoura City, Egypt. 1HNMR spectra were recorded on Varian Mercury-500 (500 MHz) (Palo Alto, CA, USA), Varian Gemini-300BB (300 MHz) (Foster City, CA, USA), and Bruker 400 MHz AV III (400 MHz) (Biocity’s, CA, USA) using dimethyl sulfoxide (DMSO)-d6 as a solvent and tetramethylsilane (TMS) as internal standard (chemical shift in δ, ppm). 13CNMR spectra were recorded on Varian Gemini-300BB (100 MHz) (Foster City, CA, USA). All reactions were monitored by thin-layer chromatography (TLC) using Silica gel 60 GF254 (E-Merck-Germany) and were visualised by iodine vapours or by UV-lamp at wavelength λ 254 nm.
3
Synthesis of 5-Bromo-3-Methyl-5H-Furan-2-One
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The common intermediate, 5-bromo-3-methyl-5H-furan-2-one 2 , was obtained with good yield by the bromination of 3-methyl-5H-furan-2-one with N-bromosuccinimide in CCl4, in the presence of benzoyl peroxide [73 (link)] and it was used as crude reaction product (94–95%).
The melting points (mp) were determined on a Boetius apparatus and are uncorrected. The IR spectra were registered on a Fourier-transform (FT)-IR Vertex 70 spectrometer (Bruker Optik GmbH, Ettlingen, Germany) in ATR modes. The NMR spectra were recorded on a Varian Gemini 300 BB instrument, operating at 300.1 MHz and 75.5 MHz for 1H and 13C nuclei, respectively, or on a Bruker Avance III instrument, operating at 500 MHz, and 100 MHz, respectively. Chemical shifts are reported as δ (ppm) and were referenced to internal TMS for 1H chemical shifts and to the internal deuterated solvent for 13C chemical shifts (CDCl3 referenced at 77.0 ppm) and unambiguously assigned based on additional COSY, HSQC/HETCOR and HMBC experiments. The elemental analysis was carried out on a COSTECH Instruments EAS32 apparatus. Satisfactory microanalyses for all new compounds were obtained.
The melting points (mp) were determined on a Boetius apparatus and are uncorrected. The IR spectra were registered on a Fourier-transform (FT)-IR Vertex 70 spectrometer (Bruker Optik GmbH, Ettlingen, Germany) in ATR modes. The NMR spectra were recorded on a Varian Gemini 300 BB instrument, operating at 300.1 MHz and 75.5 MHz for 1H and 13C nuclei, respectively, or on a Bruker Avance III instrument, operating at 500 MHz, and 100 MHz, respectively. Chemical shifts are reported as δ (ppm) and were referenced to internal TMS for 1H chemical shifts and to the internal deuterated solvent for 13C chemical shifts (CDCl3 referenced at 77.0 ppm) and unambiguously assigned based on additional COSY, HSQC/HETCOR and HMBC experiments. The elemental analysis was carried out on a COSTECH Instruments EAS32 apparatus. Satisfactory microanalyses for all new compounds were obtained.
4
Spectroscopic Characterization of Organic Compounds
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Melting points were measured with a Stuart melting point apparatus and were uncorrected. Infrared spectra were recorded as potassium bromide discs on Schimadzu FT-IR 8400Sspectrophotometer and expressed in wave number (cm–1). The NMR spectra were recorded by Varian Gemini-300BB at 300 MHz (Varian Inc., Palo Alto, CA) or Bruker spectrophotometer at 400 MHz. 1H NMR spectra were run at 300 or 400 MHz, while 13 C NMR spectra were run at 75or 100 MHz in deuterated dimethyl sulfoxide (DMSO-d6) or deuterated chloroform (CDCl3).
Chemical shifts (δH) are reported relative to TMS as internal standard. All coupling constant (J) values are given in hertz. Chemical shifts (δC) are reported relative to DMSO-d6 as internal standard. The abbreviations used are as follows: s, singlet; d, doublet; m, multiplet. Mass spectra were measured on a GCMS-QP1000 EX and Helwett Packard 5988 spectrometers at 70 eV.
Elemental analyses were carried out at the Regional Center for Microbiology and Biotechnology, Al-Azhar University, Cairo, Egypt. Analytical thin layer chromatography on silica gel plates containing UV indicator was employed routinely to follow the course of reactions and to check the purity of products. All reagents and solvents were purified and dried by standard techniques.
Chemical shifts (δH) are reported relative to TMS as internal standard. All coupling constant (J) values are given in hertz. Chemical shifts (δC) are reported relative to DMSO-d6 as internal standard. The abbreviations used are as follows: s, singlet; d, doublet; m, multiplet. Mass spectra were measured on a GCMS-QP1000 EX and Helwett Packard 5988 spectrometers at 70 eV.
Elemental analyses were carried out at the Regional Center for Microbiology and Biotechnology, Al-Azhar University, Cairo, Egypt. Analytical thin layer chromatography on silica gel plates containing UV indicator was employed routinely to follow the course of reactions and to check the purity of products. All reagents and solvents were purified and dried by standard techniques.
5
Spectroscopic Characterization of Organic Compounds
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The melting points (m.p.) were measured in open capillary tubes on an Electrothermal 9100 apparatus and are uncorrected. The 1H-NMR and 13C-NMR spectra were recorded on a Gemini 300 BB instrument (Varian, Palo Alto, CA, USA) at room temperature, operating at 300 MHz for 1H and 75.075 MHz for 13C. The chemical shifts were recorded as δ values in ppm units downfield to tetrametylsilane (TMS) used as internal standard, and CDCl3 and DMSO-d6 as solvents. The coupling constants values (J) are reported in hertz (Hz) and the splitting patterns are abbreviated as follows: s, singlet; d, doublet; t, triplet; q, quartet; and b, broad. The carbons not attached to any protons are presented as Cq, while those attached to a hydrogen atom are designated as CH.
The IR spectra were recorded on a FT/IR-4200 spectrometer (JASCO, Tokyo, Japan) with an ATR PRO450-S accessory at a resolution of 4 cm−1. The elemental analyses were performed on a Perkin–Elmer 2400 Series II CHNS/O Elemental Analyzer (Shelton, CT, USA).
The IR spectra were recorded on a FT/IR-4200 spectrometer (JASCO, Tokyo, Japan) with an ATR PRO450-S accessory at a resolution of 4 cm−1. The elemental analyses were performed on a Perkin–Elmer 2400 Series II CHNS/O Elemental Analyzer (Shelton, CT, USA).
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