All melting points were measured on a Gallenkamp melting point apparatus. The infrared spectra were recorded in potassium bromide discs on a Pye Unicam SP 3–300 and Shimadzu FT IR 8101 PC infrared spectrophotometers. The NMR spectra were recorded in deuterated chloroform (CDCl3) or dimethyl sulfoxide (DMSO-d6). On a Varian Mercury VXR-300 NMR spectrometer. Chemical shifts were related to that of the solvent. Mass spectra were recorded on a Shimadzu GCMS-QP1000 EX mass spectrometer at 70 eV. Elemental analyses were recorded on a Elementar-Vario EL automatic analyzer at the Micro-analytical Centre of Cairo University, Giza, Egypt. Formamidine 3 is prepared according to our pervious reported work [39 (link)] (Scheme 6 ). The Microwave irradiation was carried out on a CEM mars machine. CEM has several vessel types that are designed for their ovens: Closed-system vessels including the HP-500 (500 psig material design pressure and 260 °C), pictured below, have liners are composed of PFA and are ideal for many types of samples. HP-500 Plus vessels are ideal for routine digestion applications. Process up to 14 high-pressure vessels per run with temperatures up to 260 °C or pressures up to 500 psi (Scheme 7 ).
Unicam sp 3 300
Manufactured by Shimadzu
Sourced in Japan
The Unicam SP 3–300 is a UV-Vis spectrophotometer designed for laboratory applications. It is capable of measuring the absorbance or transmittance of samples across the ultraviolet and visible light spectrum.
Automatically generated - may contain errors
Lab products found in correlation
Ft ir 8101 pc infrared spectrophotometer, by Shimadzu (7 mentions)
Mercury vxr 300 nmr spectrometer, by Agilent Technologies (3 mentions)
Gcmqp 1000 ex spectrometer, by Shimadzu (3 mentions)
Gcms qp1000 ex mass spectrometer, by Shimadzu (2 mentions)
Mercury vx 300 nmr spectrometer, by Agilent Technologies (2 mentions)
Gcms qp 1000 ex mass spectrometer, by Elementar (1 mentions)
Mercury vxr 300 nmr spectrometer, by Bruker (1 mentions)
Jnm la500 spectrometer, by JEOL (1 mentions)
Gemini 300 nmr spectrometer, by Agilent Technologies (1 mentions)
Silica gel, by Merck Group (1 mentions)
Mercury vx 400 nmr spectrometer, by Agilent Technologies (1 mentions)
Silica gel ib2 f plates, by Merck Group (1 mentions)
Ft ir 8101 pc, by Shimadzu (1 mentions)
Silica gel 60 f254, by Merck Group (1 mentions)
60 f254 aluminum sheets, by Merck Group (1 mentions)
Gc ms qp1000 ex, by Shimadzu (1 mentions)
11 protocols using unicam sp 3 300
1
Microwave-Assisted Synthesis of Formamidine Derivatives
2
Characterization of Organic Compounds
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Melting points were determined in open glass capillaries with a Gallenkamp apparatus. The infrared spectra were recorded in potassium bromide disks on a Pye Unicam SP 3-300 and Shimadzu FTIR 8101 PC infrared spectrophotometer. NMR spectra were recorded with a Varian Mercury VXR-300 NMR spectrometer operating at (300 MHz and 75 MHz) or Bruker AVS NMR spectrometer at (400 MHz and 101 MHz), respectively, using TMS as an internal standard. Chemical shifts were reported as δ values in ppm. Mass spectra (EI) were obtained at 70 eV with a type Shimadzu GCMQP 1000 EX spectrometer. Analytical thin-layer chromatography was performed using pre-coated silica gel 60 778 plates (Fluka), and the spots were visualized with UV light at 254 nm. Elemental analyses were performed on a Perkin-Elmer 240 micoanalyser at the Micro analytical Center of Cairo University. All chemicals were purchased from Sigma-Aldrich and used without further purification.
3
Synthesis and Characterization of Novel Heterocyclic Compounds
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Melting points were determined in open glass capillaries with a Gallenkamp apparatus. Elemental analyses were carried out at the Microanalytical Center of Cairo University, Giza, Egypt. The infrared spectra were recorded as potassium bromide disks on a Pye Unicam SP 3–300 and Shimadzu FTIR 8101 PC infrared spectrophotometer. NMR spectra were recorded on Varian Mercury VXR-300 NMR spectrometer at 300 MHz (1H NMR) and at 75 MHz (13C NMR) using DMSO-d6 as solvent Chemical shifts were reported downfield from TMS (= 0) for 1H NMR. For 13C NMR, chemical shifts were reported in the scale relative to the solvent used as an internal reference. Mass spectra (EI) were obtained at 70 eV with a type Shimadzu GCMQP 1000 EX spectrometer. The enaminone 3 , [55 (link)] hydrazonoyl chloride 4 , [56 ] aldehyde-thiosemicarbazones 7a-c , [57 , 58 (link)] acetyl-thiosemicarbazones 9, 10, 11 [59 (link), 60 (link)], bis-aldehydes 15a-c , 19a-c [61 (link)–63 (link)], and bis-thiosemicarbazones 17a-c , 20a-c , [64 (link)–67 (link)] were prepared following procedures reported in the literature.
4
Microwave-Assisted Organic Synthesis Protocols
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All melting points were measured on a Gallenkamp melting point apparatus. The infrared spectra were recorded in potassium bromide discs on a Pye Unicam SP 3–300 and Shimadzu FT IR 8101 PC infrared spectrophotometers. The NMR spectra were recorded in dimethyl sulfoxide (DMSO-d6) or CDCl3.on a Varian Mercury VXR-300 NMR spectrometer. Chemical shifts were related to that of the solvent. Mass spectra were recorded on a Shimadzu GCMS-QP1000 EX mass spectrometer at 70 eV. The Microwave irradiation was carried out on a CEM mars machine. CEM has several vessel types that are designed for their ovens: closed-system vessels including the HP-500 (500 psig material design pressure and 260 °C), have liners are composed of PFA and are ideal for many types of samples. HP-500 Plus vessels are ideal for routine digestion applications. Process up to 14 high-pressure vessels per run with temperatures up to 260 °C or pressures up to 500 psi.
5
Analytical Characterization of Chemical Compounds
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Melting points were determined
in open glass capillaries with a
Gallenkamp apparatus. Elemental analyses were carried out at the Microanalytical
Center of Cairo University, Giza, Egypt. Infrared spectra were recorded
as potassium bromide disks on a Pye Unicam SP 3-300 and Shimadzu FTIR
8101 PC infrared spectrophotometer. NMR spectra were recorded on a
JEOL JNM-LA500 spectrometer, operating at 500 MHz for 1H NMR, and 125.65 MHz for 13C NMR. Chemical shifts were
reported downfield from TMS (= 0) for 1H NMR. For 13C NMR, chemical shifts were reported in the scale relative
to the solvent used as an internal reference. Mass spectra (EI) were
obtained at 70 eV with a type Shimadzu GCMQP 1000 EX spectrometer.
Analytical thin-layer chromatography was performed using precoated
silica gel 60,778 plates (Fluka), and the spots were visualized with
UV light at 254 nm.
in open glass capillaries with a
Gallenkamp apparatus. Elemental analyses were carried out at the Microanalytical
Center of Cairo University, Giza, Egypt. Infrared spectra were recorded
as potassium bromide disks on a Pye Unicam SP 3-300 and Shimadzu FTIR
8101 PC infrared spectrophotometer. NMR spectra were recorded on a
JEOL JNM-LA500 spectrometer, operating at 500 MHz for 1H NMR, and 125.65 MHz for 13C NMR. Chemical shifts were
reported downfield from TMS (= 0) for 1H NMR. For 13C NMR, chemical shifts were reported in the scale relative
to the solvent used as an internal reference. Mass spectra (EI) were
obtained at 70 eV with a type Shimadzu GCMQP 1000 EX spectrometer.
Analytical thin-layer chromatography was performed using precoated
silica gel 60,778 plates (Fluka), and the spots were visualized with
UV light at 254 nm.
6
Spectroscopic Characterization of Heterocyclic Compounds
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Measurements of the melting points were carried out on Electrothermal IA 9000 series digital melting point apparatus (Bibby Sci. Lim. Stone, Staffordshire, UK). The IR spectra were recorded in potassium bromide discs on a Pye Unicam SP 3300 and Shimadzu FT-IR 8101 PC infrared spectrophotometer (Shimadzu, Tokyo, Japan). 1H-NMR and 13C-NMR spectra were measured in deuterated dimethyl sulfoxide (DMSO-d6) using a Varian Gemini 300 NMR spectrometer (Varian, Inc., Karlsruhe, Germany). Mass spectra were recorded on a Shimadzu GCMS-QP1000 EX mass spectrometer (Tokyo, Japan) at 70 eV. Measurements of the elemental analysis were carried out at the Microanalytical Centre of Cairo University, Giza, Egypt. All reactions were followed by TLC (Silica gel, Merck, Kenilworth, NJ, USA). The biological evaluation of the products was carried out at the Regional Center for Mycology and Biotechnology at Al-Azhar University, Cairo, Egypt. Bis-hydrazonoyl chloride 1 [24 (link)] and the methyl arylidene dithiocarbamate 2 , 6 , 8 [25 (link),26 (link),27 (link),28 (link)] were prepared as described in the literature.
7
Spectroscopic Characterization of Organic Compounds
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1H NMR spectra were run at 400 MHz and 13 C NMR spectra were determined at 101 MHz in deuterated dimethyl sulfoxide (DMSO-d6) on a Varian Mercury VX-400 NMR spectrometer. Chemical shifts are given in parts per million (ppm) on the delta (d) scale. Chemical shifts were calibrated relative to those of the solvents. The progress of reactions was monitored with Merck silica gel IB2-F plates (0.25 mm thickness). The infra-red spectra were recorded in potassium bromide discs on Pye Unicam SP 3300 and Shimadzu FT IR 8101 PC infra-red spectrophotometer. Elemental analyses (C, H, N) were performed on a CHN analyser, and all compounds were within ± 0.4 of the theoretical values. Compounds 2 , 3 , 4 , and 5 were prepared according to reported procedures 44–46 (link).
8
Synthesis and Characterization of Novel Compounds
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Melting points were measured using an Electrothermal IA 9100 equipment with open capillary tube and were kept uncorrected. All experiments were done using dry solvents. TLC was performed on Merck Silica Gel 60F254 with detection by way of UV Light. The formed compound has been purified using recrystallization. The IR spectra (KBr disc) were recorded using Pye Unicam Sp-3-300 or a Shimadzu FTIR 8101 PC infrared spectrophotometer. The 1H NMR and 13C NMR spectra were measured by means of JEOL-JNM-LA 400 MHz spectrometer using DMSO-d6 as a solvent. All chemical shifts had been expressed on the δ (ppm) scale using TMS as an internal well-known reference. The coupling constant (J) values are given in Hz. Analytical information was acquired from the Microanalysis center at Cairo University, Giza, Egypt.
9
Synthesis and Characterization of Hydrazonoyl Chlorides
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All melting points were measured on Electrothermal IA 9000 series digital melting point apparatus. The IR spectra were recorded in potassium bromide disks on a Pye Unicam SP 3300 and Shimadzu FT IR 8101 PC infrared spectrophotometer. 1H NMR (300 MHz) was run in deuterated dimethyl sulfoxide (DMSO-d6). Chemical shifts were related to that of the solvent. Mass Spectra were recorded on a Shimadzu GCMS-QP1000 EX mass spectrometer at 70 eV. Elemental analyses were carried out at the Microanalytical Center of Cairo University, Giza, Egypt. All reactions were followed by TLC (Silica gel, Aluminum Sheets 60 F254, Merck). 2-(2-benzoylhydrazono)-N′-phenylpropanehydrazonoyl chloride 6a , 2-(2-benzoylhydrazono)-N′-p-tolylpropanehydrazonoyl chloride 6b , 2-(2-(4-methylbenzoyl)hydrazono)-N′-(p-tolyl)propanehydrazonoyl chloride 6c, methyl N-phenyldithiocarbamate, methyl benzylidenedithiocarbazate, methyl dithiocarbazate, methyl benzoylcarbodithioate, and 5-phenyl-1,3,4-oxadiazole-2-thiol were prepared as reported in the literature [18] , [19] , [23] , [24] .
10
Comprehensive Characterization of Compound
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The melting point was measured by a Gallenkamp electrothermal melting point apparatus. The infrared spectrum was recorded for potassium bromide on a Pye Unicam Sp 3-300 and Shimadzu FT IR 8101 PC infrared spectrophotometer. The NMR spectrum was recorded on a Varian Mercury VX-300 NMR spectrometer. 1 H spectrum was run at 300 MHz. Chemical shifts are quoted in δ and were related to that of the solvents. The oil oxidative stability was estimated by measuring the oxidation induction time on a Rancimat apparatus (Metrohm CH series 679) . Air (20 L/h was bubbled through the oil (5.0 g) heated at 100±2℃ with the volatile compounds being collected in water, and the increasing water conductivity was continually measured. The time taken to reach the conductivity inflection was recorded 4) .
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