Chemical reagents and solvent required during the synthesis process were purchased from Energy Chemical and were used and purified according to standard methods. Bruker AM-400 (Bruker Company, USA) spectrometer was employed to obtain 1H NMR (400 MHz) and 13 C NMR (100 MHz) spectra of new derivatives and TMS was used as reference. ZAB-HS and Bruker Daltonics APEXII49e instruments were used to obtain electrospray ionisation mass spectrometry. A Kofler melting point apparatus was used to detect melting points of the new derivatives. The purity of synthesised compound was confirmed by high performance liquid chromatography (VARIAN, ProStar) equipped with an Ultimate XB-C18 column and eluted with methanol-water containing 0.1% TFA at a flow rate of 1 ml/min.
Apexii49e
Manufactured by Bruker
The APEXII49e is a high-performance, ultra-high field Fourier transform ion cyclotron resonance (FT-ICR) mass spectrometer designed for advanced analytical applications. It features a 9.4 Tesla superconducting magnet and is capable of delivering high-resolution, high-mass accuracy mass spectra.
Automatically generated - may contain errors
4 protocols using apexii49e
1
Synthesis and Characterization of New Derivatives
2
Isolation and Purification of Compound 1
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N-Boc-amino
acids and TFA were purchased from GL Biochem (Shanghai) Company. DIPC
and DMAP were purchased from Sigma Chemical Company (China). Other
reagents and solvents were purchased from commercial sources and were
used as received. The starting compound1 was isolated
from the Chinese medicinal plant C. acuminata and
was purified before being used (>98% pure). Analytical thin-layer
chromatography (TLC) and preparative thin-layer chromatography (PTLC)
were performed with silica gel plates using silica gel 60 GF254 (Qingdao
Haiyang Chemical Co., Ltd.). Melting points were taken on a Kofler
melting point apparatus and are uncorrected. IR spectra were obtained
on an NIC-5DX spectrophotometer. MS analyses were performed on ZAB-HS
and Bruker Daltonics APEXII49e instruments. NMR spectra were recorded
on a Bruker AM-400 spectrometer at 400 MHz using TMS as reference
(Bruker Company, USA). The purity of all tested compounds was determined
by HPLC (Agilent Technologies 1100 series) equipped with a C-18 bound-phase
column (Eclipse Plus C18, 5 μM particle size, 4.6 mm ×
250 mm). A gradient elution was performed with MeOH and water as a
mobile phase and was monitored at 254 nm. All tested compounds were
>95% pure.
acids and TFA were purchased from GL Biochem (Shanghai) Company. DIPC
and DMAP were purchased from Sigma Chemical Company (China). Other
reagents and solvents were purchased from commercial sources and were
used as received. The starting compound
from the Chinese medicinal plant C. acuminata and
was purified before being used (>98% pure). Analytical thin-layer
chromatography (TLC) and preparative thin-layer chromatography (PTLC)
were performed with silica gel plates using silica gel 60 GF254 (Qingdao
Haiyang Chemical Co., Ltd.). Melting points were taken on a Kofler
melting point apparatus and are uncorrected. IR spectra were obtained
on an NIC-5DX spectrophotometer. MS analyses were performed on ZAB-HS
and Bruker Daltonics APEXII49e instruments. NMR spectra were recorded
on a Bruker AM-400 spectrometer at 400 MHz using TMS as reference
(Bruker Company, USA). The purity of all tested compounds was determined
by HPLC (Agilent Technologies 1100 series) equipped with a C-18 bound-phase
column (Eclipse Plus C18, 5 μM particle size, 4.6 mm ×
250 mm). A gradient elution was performed with MeOH and water as a
mobile phase and was monitored at 254 nm. All tested compounds were
>95% pure.
3
Spectroscopic Characterization of BLG28
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1H NMR (400 MHz) and 13C NMR (100 MHz) spectra were recorded with a Bruker AM-400 (Bruker Company, Billerica, MA, USA) spectrometer at 400 and 101 MHz, respectively, and TMS was used as internal standard. Electrospray ionization mass spectrometry was recorded on ZAB-HS and Bruker Daltonics APEXII49e instruments. Melting point (mp) was determined using a Kofler melting point apparatus. The purity of BLG28 was confirmed by analytical HPLC (VARIAN, ProStar) with an Ultimate XB-C18 column (methanol:water 80:20, 0.1% TFA, 1 mL/min). All chemical reagents used in the synthesis process were purchased from Energy Chemical. All of the solvents were purified according to standard methods.
4
Synthesis and Characterization of N-(1-oxyl-2,2,6,6-tetramethyl-4-piperidinyloxycarbonyl)-amino Acids
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