All chemicals were provided by Enamine Ltd. (www.enamine.net ). All solvents were treated according to standard methods. All reactions were monitored by thin-layer chromatography (TLC) and were visualized using UV light. Product purification was performed using silica gel column chromatography. TLC characterization was performed with precoated silica gel GF254 (0.2 mm), while column chromatography characterization was performed with silica gel (100-200 mesh). 1H NMR spectra were recorded at 400, 500, or 600 MHz (Varian); 19 F NMR spectra were recorded at 376 MHz (Varian); and 13 C NMR spectra were recorded at 100, 126, or 151 MHz (Varian). 1H NMR chemical shifts are calibrated using residual undeuterated solvents CHCl3 (δ = 7.26 ppm) or DMSO (δ = 2.50 ppm). 13 C NMR chemical shifts for 13 C NMR are reported relative to the central CHCl3 (δ = 77.16 ppm) or DMSO (δ = 39.52 ppm). 19 F NMR chemical shifts are calibrated using CFCl3 as an internal standard. Coupling constants are given in Hz. High-resolution mass spectra (HRMS) were recorded on an Agilent LC/MSD TOF mass spectrometer by electrospray ionization time-of-flight reflectron experiments.
Lc msd tof mass spectrometer
Manufactured by Agilent Technologies
Sourced in United States
The LC/MSD TOF mass spectrometer is a high-performance analytical instrument designed for accurate mass measurements and identification of unknown compounds. It combines a liquid chromatography (LC) system with a time-of-flight (TOF) mass spectrometer, providing precise mass analysis of complex samples.
Automatically generated - may contain errors
Lab products found in correlation
19f nmr spectra, by Agilent Technologies (2 mentions)
13c nmr spectra, by Agilent Technologies (2 mentions)
Rotary evaporator, by Heidolph (1 mentions)
Ethyl acetate, by Beijing Chemical Works (1 mentions)
400 spectrometer, by Bruker (1 mentions)
Dpx 200 spectrometer, by Bruker (1 mentions)
Silica gel 60, by Merck Group (1 mentions)
Lc 1100 series, by Agilent Technologies (1 mentions)
I class lc, by Waters Corporation (1 mentions)
10 protocols using lc msd tof mass spectrometer
1
Comprehensive Organic Synthesis Protocol
2
Synthesis and Characterization of Terminal Alkenes
3
Synthesis of 5-Alkyl-6-(cyclohexylmethyl)-2-thioxo-2,3-dihydropyrimidin-4(1H)-one Derivatives
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Melting points (m.p.) were determined by a WRS-1 digital melting point instrument (Shanghai, China). 1H NMR and 13C NMR spectra were obtained on a Bruker AM 400/300 MHz spectrometer (Fällanden, Switzerland) using dimethyl sulfoxide-d6 (DMSO-d6) as solvent. Chemical shifts are reported in δ (ppm) units relative to the internal reference tetramethylsilane (TMS). Mass spectra were obtained on an Agilent LC/MSD TOF mass spectrometer (Watertown, MA, USA). The regents and solvents used were all of analytical grades, and were purified and dried by standard methods before use. All air-sensitive reactions were run under nitrogen stream protection. All the reactions were monitored by thin-layer chromatography (TLC) on pre-coated silica gel G plates at 254 nm under a UV lamp using ethyl acetate/petroleum ether as eluents. Flash chromatography separations were obtained on silica gel (300–400 mesh; Qingdao Marine Chemical Factory, Qingdao, China). 5-Alkyl-6-(cyclohexylmethyl)-2-thioxo-2,3-dihydropyrimidin-4(1H)-one (4 ) was prepared as previously reported25 (link),27 .
4
Synthesis and Characterization of Organic Compounds
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All chemicals were provided
by Enamine Ltd. (www.enamine.net ). All solvents were treated according to standard methods. All reactions
were monitored by thin-layer chromatography (TLC) and were visualized
using UV light. Product purification was performed using silica gel
column chromatography. TLC characterization was performed with precoated
silica gel GF254 (0.2 mm), while column chromatography characterization
was performed with silica gel (100–200 mesh). 1H
NMR spectra were recorded at 400, 500, or 600 MHz (Varian); 19F NMR spectra were recorded at 376 MHz (Varian); and 13C NMR spectra were recorded at 100, 126, or 151 MHz (Varian). 1H NMR chemical shifts are calibrated using residual undeuterated
solvents CHCl3 (δ = 7.26 ppm) or DMSO (δ =
2.50 ppm). 13C NMR chemical shifts for 13C NMR
are reported relative to the central CHCl3 (δ = 77.16
ppm) or DMSO (δ = 39.52 ppm). 19F NMR chemical shifts
are calibrated using CFCl3 as an internal standard. Coupling
constants are given in Hz. High-resolution mass spectra (HRMS) were
recorded on an Agilent LC/MSD TOF mass spectrometer by electrospray
ionization time-of-flight reflectron experiments.
by Enamine Ltd. (
were monitored by thin-layer chromatography (TLC) and were visualized
using UV light. Product purification was performed using silica gel
column chromatography. TLC characterization was performed with precoated
silica gel GF254 (0.2 mm), while column chromatography characterization
was performed with silica gel (100–200 mesh). 1H
NMR spectra were recorded at 400, 500, or 600 MHz (Varian); 19F NMR spectra were recorded at 376 MHz (Varian); and 13C NMR spectra were recorded at 100, 126, or 151 MHz (Varian). 1H NMR chemical shifts are calibrated using residual undeuterated
solvents CHCl3 (δ = 7.26 ppm) or DMSO (δ =
2.50 ppm). 13C NMR chemical shifts for 13C NMR
are reported relative to the central CHCl3 (δ = 77.16
ppm) or DMSO (δ = 39.52 ppm). 19F NMR chemical shifts
are calibrated using CFCl3 as an internal standard. Coupling
constants are given in Hz. High-resolution mass spectra (HRMS) were
recorded on an Agilent LC/MSD TOF mass spectrometer by electrospray
ionization time-of-flight reflectron experiments.
5
Melting Point and Spectroscopic Analysis
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Melting points were determined on a WRS-1 digital melting point apparatus and are calibrated. 1H NMR and 13C NMR spectra were obtained on a Brucker AM 400 MHz spectrometer in the indicated solvents. Chemical shifts are expressed in δ units and TMS as internal reference. Mass spectra were taken on an Agilent LC/MSD TOF mass spectrometer. Solvents were reagent quality and, when necessary, were purified and dried by typical methods. Concentration of the reaction solutions involved the use of rotary evaporator (Heidolph) at reduced pressure. TLC was performed on silica gel GF254 for TLC (Shanghai Haohong Biopharmaceutical Technology Co., Ltd., Shanghai, China) and spots were visualized by iodine vapors or by irradiation with UV light (254 nm).
6
Analytical Characterization of Organic Compounds
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Melting points were measured on a Yanaco MP-500 melting point apparatus (Yanaco Ltd., Osaka, Japan) and are uncorrected. 1H-NMR and 13C-NMR spectra were recorded with a Bruker 400 spectrometer (Bruker Company, Billerica, MA, USA) in CDCl3 with tetramethylsilane (TMS) as an internal standard, or in D2O with DOH as an internal standard in 1H-NMR, or with HCO2H (166.3 ppm) as an internal standard in 13C-NMR. IR spectra were obtained on a Nicolet AVATAR 330 FTIR spectrometer (Thermo Nicolet Corporation, Madison, WI, USA). HRMS spectra were recorded with a Liquid Chromatography/Mass Spectrometry/Data and Time-of-Flight (LC/MSD TOF) mass spectrometer (Agilent, Santa Clara, CA, USA). TLC analysis was performed on glass pre-coated silica gel YT257‒85 (10‒40 µm) plate (Qingdao Ocean Chemical Industry, Qingdao, China). Spots were visualized with UV light or iodine. Column chromatography was performed on silica gel zcx II (200‒300 mesh) (Qingdao Ocean Chemical Industry, Qingdao, China) with petroleum-ether (PE) and ethyl-acetate (EA) (Beijing Chemical Reagent Company, Beijing, China) as the eluent.
7
Boc-Glu(OBzl) Synthesis and Characterization
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All reagents used were commercial
products and were used without further purification unless otherwise
indicated. Boc-Glu(OBzl)–OH (Boc-l -glutamic acid 5-benzyl
ester,15 ) was purchased from Sigma-Aldrich. Flash chromatography
(FC) was performed using silica gel 60 (230–400 mesh, Sigma-Aldrich). 1H NMR spectra were obtained at 200 MHz and 13C
NMR spectra were recorded at 50 MHz (Bruker DPX 200 spectrometer).
Chemical shifts are reported as δ values (parts per million)
relative to remaining protons in deuterated solvent. Coupling constants
are reported in hertz. The multiplicity is defined by s (singlet),
d (doublet), t (triplet), q (quartet), p (pentet), br (broad), or
m (multiplet). HPLC analyses were performed on an Aglient LC 1100
series. High-resolution MS experiments were performed using an Agilent
Technologies LC/MSD TOF mass spectrometer.
products and were used without further purification unless otherwise
indicated. Boc-Glu(OBzl)–OH (Boc-
ester,
(FC) was performed using silica gel 60 (230–400 mesh, Sigma-Aldrich). 1H NMR spectra were obtained at 200 MHz and 13C
NMR spectra were recorded at 50 MHz (Bruker DPX 200 spectrometer).
Chemical shifts are reported as δ values (parts per million)
relative to remaining protons in deuterated solvent. Coupling constants
are reported in hertz. The multiplicity is defined by s (singlet),
d (doublet), t (triplet), q (quartet), p (pentet), br (broad), or
m (multiplet). HPLC analyses were performed on an Aglient LC 1100
series. High-resolution MS experiments were performed using an Agilent
Technologies LC/MSD TOF mass spectrometer.
8
General Synthetic Procedures and Analytical Methods
9
Synthesis of Diazosulfamoylacetamides
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Toluene was refluxed over Na with diphenyl ketone as an indicator and freshly distilled prior to use. Melting points were obtained on a MP-500 melting point apparatus and are uncorrected. 1H and 13C-NMR spectra were recorded on a 400 MHz Bruker spectrometer in CDCl3 with TMS as an internal standard and the chemical shifts (δ) are reported in parts per million (ppm). The IR spectra (KBr pellets, v (cm−1)) were taken on a FTIR spectrometer. HRMS measurements were carried out on an Agilent LC/MSD TOF mass spectrometer. TLC separations were performed on silica gel GF254 plates, and the plates were visualized under UV light. Petroleum ether (PE, 30−60 °C) and ethyl acetate (EA) were used for column separation.
It is noteworthy that the signal of the carbon attached with diazo group in diazosulfamoylacetamides1 cannot be displayed in their 13C-NMR spectra. Similar observations were also reported by Novikov and Du Bios in the synthesis of diazosulfones and diazosulfonates, respectively [27 (link),28 (link)].
It is noteworthy that the signal of the carbon attached with diazo group in diazosulfamoylacetamides
10
Antibody Reduction and Analysis
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Antibodies were reduced in 10 mM (tris(2-carboxyethyl)phosphine), 0.1% formic acid, at pH 3 for 30 min at 55 C before injection. Reduced HC and light chain (LC) were separated by RP-HPLC at 80 C on a RP-diphenyl column (2 Â 100 mm, Waters), in trifluoroacetic acid with a linear acetonitrile gradient of 1%/min. The flow rate was maintained at 400 mL/min. Peak elution was monitored by both UV 220 nm and electrospray ionization MS on an LC-MSD-TOF mass spectrometer (Agilent Technologies). The ionization voltage was set at 5 kV, with a scan range set at 300-4000 mass units. Mass determinations were performed on MassHunter Analysis deconvolution software (Agilent Technologies).
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