OXFORD NMR S400, Varian Mercury Plus 400, Oxford, United Kingdom, equipped with workstation Sun Blade 150, software VNMRJ 1.1d, and operating system Solaris 9. 1H NMR analyses were recorded at 400 MHz and 13C NMR analyses were recorded at 100 MHz. Ir spectra were recorded with a Spectrum Two FT-IR spectrometer, Waltham, MA, United States equipped with ZnSe window, Dynascan Interferometer, detector type LiTaO3, and Spectrum 10 software. Microanalyses were performed with a CHNS-O analyzer Model EA 1108 from Fisons Instruments. GS-MS analyses were obtained on an Agilent GC(6850N)/MS(5973N), Stevens Creek Blvd, Santa Clara, CA, United States, EI technique (70 eV), GC/MSD software, and an HP-5MS column, 30 m, Id 0.25 µm, film thichness 0.25 µm. Microwave irradiations were performed by means of a Biotage® Initiator+ from Biotage, Uppsala, Sweden. Compound 3j is known, and its spectroscopic data are in agreement with those reported in the literature [21 (link)].
Initiator
Manufactured by Biotage
Sourced in Sweden, Austria
The Initiator is a laboratory equipment product by Biotage. It is a microwave synthesis system used for efficient chemical reactions and syntheses. The Initiator utilizes microwave technology to heat and control reaction conditions, enabling rapid and reproducible results.
Automatically generated - may contain errors
Lab products found in correlation
Avance 400, by Bruker (3 mentions)
Elix deionizer, by Merck Group (2 mentions)
Progard s2 ion exchange resins, by Merck Group (2 mentions)
Optima 3000 sd spectrometer, by PerkinElmer (2 mentions)
Branson sfx250 sonicator, by Emerson (2 mentions)
Microtof q 2, by Bruker (2 mentions)
Microtof q 2 spectrometer, by Bruker (2 mentions)
Mercury plus 400, by Agilent Technologies (1 mentions)
Milli q water purification system, by Merck Group (1 mentions)
Zorbax eclipse xdb c18, by Agilent Technologies (1 mentions)
Eclipse plus c18, by Agilent Technologies (1 mentions)
Hplc grade solvents, by Thermo Fisher Scientific (1 mentions)
60 f254 plate, by Merck Group (1 mentions)
Drx 400 mhz, by Bruker (1 mentions)
Micromass q tof mass spectrometer, by Waters Corporation (1 mentions)
Eclipse xdb c18 column, by Agilent Technologies (1 mentions)
Avance 500 mhz nmr spectrometer, by Bruker (1 mentions)
P 1010 polarimeter, by Jasco (1 mentions)
400 mhz nmr spectrometer, by Bruker (1 mentions)
500 mhz system, by Bruker (1 mentions)
43 protocols using initiator
1
Characterization of Compound 3j
2
Microwave-Assisted Organic Synthesis Protocols
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
All reagents and solvents were obtained from commercial suppliers and used without further purification. High purity water used in the synthetic procedures and HPLC experiments was obtained from a Milli-Q water purification system (Millipore GmbH, Vienna, Austria). Microwave-assisted experiments were carried out in a Biotage® Initiator + (Biotage AB, Uppsala, Sweden) single-mode microwave instrument producing controlled irradiation at 2.45 GHz in Pyrex microwave reaction vials. The vials were equipped with magnetic stirring bars and magnetic stirring at a rate of 720 rpm was used throughout the experiments. Reaction times refer to hold times at the temperatures indicated, not to total irradiation times. The temperature was measured with an IR sensor on the outside of the reaction vessel. HPLC analyses were performed on Agilent 1200 series, equipped with Agilent Zorbax Eclipse XDB-C18 (4.6 × 150 mm, 5 µm) column at 25 °C, a flow rate of 1.0 ml min -1 and UV-Vis detection. Mobile phase consisted of 0.1% Bu 4 NCl in water/MeOH mixtures; stepwise gradient elution (e.g., 35% MeOH for 14 min, followed by 60% MeOH for 4 min) was used. High resolution mass spectra (HRMS) were
3
Microwave-Assisted Chitin Depolymerization
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
The microwave-assisted conversion of chitin to 5-HMF was carried out using microwave reaction vials. In a typical experimental run, 25 mg of chitin, 5 mL of solvent (H2O : DMSO = 1 : 4) and 100 mg catalysts were putted into a 10 mL reactor. After being sealed with a cap, the reactor containing the mixture was mounted in a microwave reactor apparatus (Biotage Initiator+) and heated at a specified reaction time under magnetic stirring. Time zero of the reaction was defined as the time when the reactor reached its set point temperature. Reactions were performed in triplicate to assess the reproducibility of results. The liquids and solid residues were separated by filtration. The liquid sample was collected after reaction and the concentration of the product species were quantified using Agilent Technologies HPLC with a ZORBAX Eclipse Plus C18 as the analytical column and both RID (refractive index) and VWD (UV-Vis) detectors. The HPLC was operated under the following conditions: oven temperature as 35 °C, mobile phase as 5 mM H2SO4; flow rate of 0.6 mL min−1; injection volume of 5 μL. The concentrations of NAG, LA, FA, AA and 5-HMF were quantified through the external standard method and calibration curves of commercially available standard substrates.
4
Peptide Synthesis Using Initiator+ and SPPS
5
Preparative HPLC Purification of Glucuronides
6
Synthesis of Compound 3 via Palladium-Catalyzed Coupling
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
Example 81
To a solution of the compound 1 (200 mg), the compound 2 (113 mg), an dichlorobis(triphenylphosphine)palladium (24 mg) in dioxane (4 mL) was added a 2 mol/L aqueous solution of sodium carbonate (1.3 mL). The reaction mixture was stirred for 20 minutes at 170° C. in a microwave reactor (Initiator, manufactured by Biotage Inc.) The reaction mixture was cooled to room temperature, and a saturated aqueous solution of sodium carbonate was added thereto. Then, the reaction mixture was extracted with chloroform. The organic layer was washed twice with saturated brine, and dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure, then the resultant residue was purified by silica gel column chromatography (eluent: ethyl acetate-methanol; gradient: 100:0-90:10) to give the compound 3 (188 mg) as a colorless solid.
MS (APCI) 358 [M+H]+
7
Synthesis of Heterocyclic Compounds
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
Example 14
(1) To a mixed solution of the compound 1 (149 mg), the compound 2 (114 mg), and dichlorobis(triphenylphosphine)palladium (18 mg) in dioxane (2 mL) was added a 2 mol/L aqueous solution of sodium carbonate (1.5 mL). The reaction mixture was stirred for 15 minutes at 150° C. in a microwave reactor (Initiator, manufactured by Biotage Inc.) The reaction mixture was cooled to room temperature, diluted with ethyl acetate, washed with water, and dried over Chem Elut (registered trademark). The solvent was distilled off under reduced pressure, and the resultant residue was purified by silica gel column chromatography (eluent: hexane-ethyl acetate; gradient: 50:50-20:80) to give the compound 3 (190 mg) as a colorless solid.
MS (APCI) 410 [M+H]+
(2) To a solution of the compound 3 (182 mg) in dichloromethane (2 mL) was added trifluoroacetic acid (1 mL) under ice cooling, and the reaction mixture was stirred for 2 hours at room temperature. The reaction mixture was diluted with methanol, and treated with packed strong cation exchange resin (PoraPak Rxn Cx, eluent: ammonia (1 mol/L methanol solution), and the eluate was concentrated under reduced pressure to give the compound 4 (142 mg) as a yellow solid.
MS (APCI) 310 [M+H]+
8
Synthesis and Characterization of Organic Compounds
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
All solvents were well-dried before use according to standard methods, and commercial reagents were directly used without further purification. TLC was performed on silica-gel 60 F254 aluminum sheets (Merck) with detection by UV and/or 10% sulfuric acid in ethanol. The purification of compounds was carried out by silica-gel column chromatography. A microwave reaction was performed in the Biotage Initiator+. 1H NMR, 13C NMR, 2D COSY, HMQC, and HMBC spectra were obtained via the Bruker DRX 400 MHz or Bruker DRX 500 MHz spectrometer at ambient temperature using CDCl3, DMSO-d6 or CD3OD as a solvent. HRMS was recorded using the Waters Micromass Q-TOF mass spectrometer.
All the final compounds were of >95% purity according to the HPLC analysis (Agilent Series 1100 system, Zorbax Eclipse XDB-C18 column, and H2O–MeCN gradient 5–95% with 0.1% TFA).
All the final compounds were of >95% purity according to the HPLC analysis (Agilent Series 1100 system, Zorbax Eclipse XDB-C18 column, and H2O–MeCN gradient 5–95% with 0.1% TFA).
9
Synthesis and Characterization of Chiral Compounds
10
Microwave-Assisted Synthesis of Sulfonamides
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
To a microwave vial containing a solution
of sulfonamide (1.0 equiv) in DMF (0.3 M) was added amine/amino alcohol
(1.05–1.2 equiv). The reaction vessel was capped and heated
in a Biotage Initiator microwave at 130 °C for 30–40 min,
after which conversion of starting material was monitored by TLC.
To the crude mixture was added Cs2CO3 (2.5 equiv),
and the mixture underwent microwave irradiation again at 150 °C
for 30–50 min. Water was added to the crude mixture, which
was extracted with EtOAc (4×). The organic layer was separated,
and the combined organic layers were washed with water and brine,
dried (Na2SO4), and concentrated under reduced
pressure to afford the crude product, which was purified by the automated
flash column chromatography system.
of sulfonamide (1.0 equiv) in DMF (0.3 M) was added amine/amino alcohol
(1.05–1.2 equiv). The reaction vessel was capped and heated
in a Biotage Initiator microwave at 130 °C for 30–40 min,
after which conversion of starting material was monitored by TLC.
To the crude mixture was added Cs2CO3 (2.5 equiv),
and the mixture underwent microwave irradiation again at 150 °C
for 30–50 min. Water was added to the crude mixture, which
was extracted with EtOAc (4×). The organic layer was separated,
and the combined organic layers were washed with water and brine,
dried (Na2SO4), and concentrated under reduced
pressure to afford the crude product, which was purified by the automated
flash column chromatography system.
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!