Unless otherwise described, all commercial reagents and solvents were purchased from commercial suppliers and used without further purification. All reactions were performed under a N2 atmosphere in flame-dried glassware. Reactions were monitored using TLC with 0.25 mm E. Merck precoated silica gel plates (60 F254). Reaction progress was monitored using TLC analysis using a UV lamp, ninhydrin, or p-anisaldehyde stain for detection purposes. All solvents were purified using standard techniques. Purification of reaction products was carried out using silica gel column chromatography with Kieselgel 60 Art. 9385 (230–400 mesh). Purities of all compounds were ≥95%, and mass spectra and purities of all compounds was accessed using Waters LC/MS system (Waters QDA Detector, Waters 2998 Photodiode Array Detector, Waters SFO System Fluidics Organizer, Water 2545 Binary Gradient Module, Waters 2767 Sample Manager) using SunFire C18 column (4.6 × 50 mm, 5 μm particle size): solvent gradient = 30% B at 0.00 min, 30% B at 1.00 min, 100% B at 7.00 min, 100% B at 8.00 min, 30% B at 8.01 min, 30% B at 10.00 min. Solvent A = 0.1% HCOOH in H2O; Solvent B = 0.1% HCOOH in MeOH; flow rate = 0.8 mL/min. 1H and 13C NMR spectra were obtained using Bruker 400 MHz FT-NMR (400 MHz for 1H, and 100 MHz for 13C) spectrometer. Standard abbreviations are used for denoting the signal multiplicities.
Waters 2767 sample manager
Manufactured by Waters Corporation
Sourced in Japan
The Waters 2767 Sample Manager is a high-performance liquid chromatography (HPLC) sample management system designed for automated sample handling and injection. It offers precise and reliable sample processing for analytical applications.
Automatically generated - may contain errors
Lab products found in correlation
Sfo system fluidics organizer, by Waters Corporation (4 mentions)
Waters 2998 photodiode array detector, by Waters Corporation (3 mentions)
Waters 515 hplc pump, by Waters Corporation (3 mentions)
2535 quaternary gradient module, by Waters Corporation (2 mentions)
Waters 3100 mass detector, by Waters Corporation (2 mentions)
Waters 2545 binary gradient module, by Waters Corporation (2 mentions)
Water 2545 binary gradient module, by Waters Corporation (1 mentions)
400 mhz ft nmr, by Bruker (1 mentions)
1260 infinity hplc system, by Thermo Fisher Scientific (1 mentions)
Lcq decaxp ms detector, by Thermo Fisher Scientific (1 mentions)
1525 binary hplc pump, by Waters Corporation (1 mentions)
Trifluoroacetic acid tfa, by Thermo Fisher Scientific (1 mentions)
Milli q apparatus, by Merck Group (1 mentions)
Amino acids, by Peptide Institute (1 mentions)
Chiralpak ia, by Daicel (1 mentions)
Sunfiretm c18 column, by Waters Corporation (1 mentions)
Inova 400, by Agilent Technologies (1 mentions)
Waters 2489 uv visible detector, by Waters Corporation (1 mentions)
Waters lc ms system, by Waters Corporation (1 mentions)
3100 mass detector, by Waters Corporation (1 mentions)
7 protocols using waters 2767 sample manager
1
General Organic Synthesis Protocol
2
Biophysical Characterization of Biomolecules
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
In-gel fluorescence scanning was performed using a Typhoon 9410 variable mode imager (excitation 532 nm, emission 580 nm). Isothermal titration calorimetry measurements were performed on a MicroCal iTC200 titration calorimeter (Malvern Instruments, United Kingdom). Peptides were purified on a preparative HPLC system with Waters (Milford, MA) 2535 Quaternary Gradient Module, Waters 515 HPLC pump, Waters SFO System Fluidics Organizer, and Waters 2767 Sample Manager. Enzymatic reactions were monitored by an LC-MS system with Waters 1525 Binary HPLC Pump, Waters 2998 Photodiode Array Detector, and Waters 3100 Mass Detector. Detection of O-Cr-ADPR was carried out by Agilent (Santa Clara, CA) 1260 Infinity HPLC system connected to a Thermo Fisher Scientific LCQ DecaXP MS detector.
3
Peptide Synthesis Purification and Analysis
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
Amino acids and protected Amino acids were purchased from PEPTIDE INSTITUTE, Inc. (Osaka, Japan). Acetonitrile (HPLC grade) for LC analysis was purchased from Wako Pure Chemical Industries, Ltd. (Osaka, Japan). Trifluoroacetic acid (TFA) was purchased from Thermo Fisher Scientific (Waltham, MA). Water was purified by a Milli-Q apparatus (Millipore Co., Milford, MA). HPLC grade solvents were used for mass spectrometric analysis; MeOH and CHCl3 (Wako Pure Chemical Industries, Ltd, Osaka, Japan).
The compounds were separated using a Unison-UK C-18 column (250 mm × 4.6 mm i.d.) (Imtakt, Co., Kyoto, Japan). Diastereomers derived from amines were separated using CHIRALPAK IA (250 mm × 4.6 mm i.d.) (Daicel Co., Osaka, Japan), when needed. An isocratic or a linear gradient elution was applied at a flow rate of 1.0 mL/min at 40 °C using water containing 0.1% TFA (solvent A) and acetonitrile containing 0.1% TFA (solvent B).
HPLC apparatus used in this study consisted of Waters 2767 Sample Manager as the injector, Waters 515 HPLC Pump as the makeup pump, Waters 2525 Binary Gradient Pump, Waters 490E Programmable Multiwavelength Detector (λ = 254 nm) (Waters Co., Milford, MA), and SSC-2120 Column Oven (Senshu Scientific Co., Ltd., Tokyo, Japan). QIT-MS was also used as a detector (see below for details).
The compounds were separated using a Unison-UK C-18 column (250 mm × 4.6 mm i.d.) (Imtakt, Co., Kyoto, Japan). Diastereomers derived from amines were separated using CHIRALPAK IA (250 mm × 4.6 mm i.d.) (Daicel Co., Osaka, Japan), when needed. An isocratic or a linear gradient elution was applied at a flow rate of 1.0 mL/min at 40 °C using water containing 0.1% TFA (solvent A) and acetonitrile containing 0.1% TFA (solvent B).
HPLC apparatus used in this study consisted of Waters 2767 Sample Manager as the injector, Waters 515 HPLC Pump as the makeup pump, Waters 2525 Binary Gradient Pump, Waters 490E Programmable Multiwavelength Detector (λ = 254 nm) (Waters Co., Milford, MA), and SSC-2120 Column Oven (Senshu Scientific Co., Ltd., Tokyo, Japan). QIT-MS was also used as a detector (see below for details).
4
Analytical Characterization of Synthetic Compounds
5
Characterization of Organic Compounds by NMR and MS
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
1H and 2D NMR experiments were recorded on a Varian Inova 750 MHz NMR spectrometer. 13C NMR spectra were recorded at 125 MHz in a Varian VNMRS-500-WB instrument (Agilent Technologies, Palo Alto, CA, USA). Chemical shifts (δ in ppm) are referenced to the carbon (δC 49.0) and residual proton (δH 3.31) signals of CD3OD. Mass spectra were obtained from a Xevo TQ mass spectrometer (Waters, Manchester, UK) connected to an ACQUITY Ultra High Performance Liquid Chromatography (UPLC) system (Waters, Manchester, UK). Purification was performed on a Waters HPLC system: Waters 2767 sample manager, Waters system fluidics organizer, Waters 2545 binary solvent manager, Waters 515 post-column HPLC pump, Waters 3100 mass detector. HRMS was acquired by Ion Trap-Time of Flight (IT-TOF) mass spectrometer instrument from Shimadzu (Kyoto, Japan)
6
Purification and Characterization of Organic Compounds
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
The intermediate compounds as well as the target compounds were purified by flash column chromatography using silica gel 60 (0.040-0.063 mm, 230-400 mesh ASTM)
and technical grade solvents. 1 H NMR and 13 C NMR analyses were carried out on a Bruker Avance 400 spectrometer using tetramethylsilane (TMS) as an internal standard. Melting points were measured on a Walden Precision Apparatus Electrothermal 9300 apparatus and were uncorrected. LC-MS analysis was conducted using the following system: Waters 2998 photodiode array detector, Waters 3100 mass detector, Waters SFO system fluidics organizer, Waters 2545 binary gradient module, Waters reagent manager, Waters 2767 sample manager, Sunfire™ C 18 column (4.6 × 50 mm, 5 μm particle size); Solvent gradient = 95% A at 0 min, 1% A at 5 min; solvent A: 0.035% trifluoroacetic acid (TFA) in water; solvent B: 0.035% TFA in MeOH; flow rate = 3.0 mL/min; the AUC was calculated using Waters MassLynx 4.1 software. The solvents and liquid reagents were transferred using hypodermic syringes. All the solvents and reagents were purchased from commercial companies, and used as such.
and technical grade solvents. 1 H NMR and 13 C NMR analyses were carried out on a Bruker Avance 400 spectrometer using tetramethylsilane (TMS) as an internal standard. Melting points were measured on a Walden Precision Apparatus Electrothermal 9300 apparatus and were uncorrected. LC-MS analysis was conducted using the following system: Waters 2998 photodiode array detector, Waters 3100 mass detector, Waters SFO system fluidics organizer, Waters 2545 binary gradient module, Waters reagent manager, Waters 2767 sample manager, Sunfire™ C 18 column (4.6 × 50 mm, 5 μm particle size); Solvent gradient = 95% A at 0 min, 1% A at 5 min; solvent A: 0.035% trifluoroacetic acid (TFA) in water; solvent B: 0.035% TFA in MeOH; flow rate = 3.0 mL/min; the AUC was calculated using Waters MassLynx 4.1 software. The solvents and liquid reagents were transferred using hypodermic syringes. All the solvents and reagents were purchased from commercial companies, and used as such.
7
Purification and Characterization of Peptides
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
All NMR spectra were recorded on a Bruker 300 or 400 MHz spectrometer. The chemical shifts were reported in ppm, and J values were reported in Hz. Peptides were purified on a Grace VYDACÒ 218TP152025 C18 column connected to a preparative-HPLC system with Waters 2535 Quaternary Gradient Module, Waters 515 HPLC pump, Waters SFO system Fluidics Organizer and Waters 2767 Sample Manager. Analytical HPLC trace after purification was obtained using a Grace VYDACÒ 218TP C18 5m column connected to an HPLC system with Agilent 1260 Infinity Quaternary Pump VL, Agilent 1260 Infinity Manual Injector and Agilent 1260 Infinity Variable Wavelength Detector. The outlet of the above HPLC system was connected to Thermo Finnigan LCQ Deca XP to obtain MS spectrums of purified peptides.
Starting materials for organic synthesis were purchased from common commercial suppliers including Sigma-Aldrich, TCI and Alfa and used without further purification. All reactions were monitored by TLC Silica gel 60 F254 from Merck. Flash column chromatography was performed with silica gel purchased from Grace (40-63 micron). All Fmoc-protected amino acids for and coupling reagents for solid phase peptide synthesis were purchased from GL Biochem (Shanghai, China).
Starting materials for organic synthesis were purchased from common commercial suppliers including Sigma-Aldrich, TCI and Alfa and used without further purification. All reactions were monitored by TLC Silica gel 60 F254 from Merck. Flash column chromatography was performed with silica gel purchased from Grace (40-63 micron). All Fmoc-protected amino acids for and coupling reagents for solid phase peptide synthesis were purchased from GL Biochem (Shanghai, China).
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!