The largest database of trusted experimental protocols

7 protocols using model 343

1

Spectroscopic Analysis of TAMCSAs

Check if the same lab product or an alternative is used in the 5 most similar protocols
NMR spectra were recorded on a Bruker Advance III spectrometer at 400 MHz for 1H NMR and 100 MHz for C NMR. NOESY experiments of TAMCSAs were completed under a number of scans (1a, 8; 1b–1d, 16), mixing time (1a–1d 0.30 s), and d1 (1a, 1.98 s; 1b, 1.82 s; 1c, 1.99 s; 1d, 1.90 s). HRMS spectra were acquired on MicrOTOF-Q II 10260, FLEX-PC, and TripleTOF 5600units. IR spectra were obtained on a Nicolet 360 Avatar IR spectrometer as KBr pellets. Optical rotations were measured with a PerkinElmer Model 343 polarimeter using the sodium D line at 589 nm. X-ray crystal structures were determined by a Smart Apex II Single Crystal diffractometer.
+ Open protocol
+ Expand
2

Monosaccharide and Fatty Acid Analysis of Capsular Polysaccharides

Check if the same lab product or an alternative is used in the 5 most similar protocols
Monosaccharides were analyzed as the alditol acetates obtained by hydrolysis of the CPS-1 (2 M CF3COOH, 120 °C, 2 h) and CPS-2 (0.5 M CF3COOH, 100 °C, 3 h) by GC on an Agilent 6850 chromatograph (Santa Clara, CA, USA) equipped with an HP-5 MS capillary column using a temperature program from 150 °C (3 min) to 230 °C (10 min) at 3 °C min−1. The absolute configurations of monosaccharides were determined by GC of the acetylated (S)-2-octyl glycosides as described [40 (link)]. The absolute configuration of d-Xlu was determined by calculation of the specific optical rotation of OS using the Klyne rule [12 (link)]. The specific optical rotation of OS was measured on a PerkinElmer instrument, model 343 (Waltham, MA, USA). Fatty acid analysis was performed by GC of methyl derivatives after methanolysis of CPS with 2 M acetylchloride in methanol (120 °C, 4 h). Proteins were analyzed by the conventional method [41 (link)].
+ Open protocol
+ Expand
3

Spectroscopic Characterization of Compounds

Check if the same lab product or an alternative is used in the 5 most similar protocols
Optical rotations were measured with Perkin Elmer/Model-343 digital polarimeter. IR spectra were recorded on a JASCO FT/IR-480 spectrophotometer and reported as wave number (cm−1). 1H, 13C NMR spectra and 2D NMR spectra were recorded on a Bruker Avance III 600 spectrometer. Chemical shifts were reported using TMS as the internal standard. HRESIMS data were obtained on a Bruker Apex IV FTMS spectrometer. Column chromatography (CC) was performed on silica gel (90 − 200 µm; Qingdao Marine Chemical Co. Ltd., Qingdao, People’s Republic of China), and MPLC was performed on a Lisui EZ Purify III System packed with RP-18 silica gel (40–63 μm, Merck, 71 Darmstadt, Germany) columns. Precoated silica gel GF254 plates (Qingdao Marine Chemical Co. Ltd., Qingdao, People’s Republic of China) were used for thin-layer chromatography (TLC). Preparative HPLC was performed on Shimadzu LC-8A equipped with a Shimadzu PRC-ODS(K) column and Agilent 1100 apparatus equipped with a Zorbax SB-C-1875 (Agilent, 9.4 mm × 25 cm) column, respectively. The reagents were purchased from Fisher Scientific at the highest quality and were used without further purification.
+ Open protocol
+ Expand
4

Optical Rotation of Isopulegol Enantiomers

Check if the same lab product or an alternative is used in the 5 most similar protocols

EXAMPLE 1

Rotation value measurements were performed for the system L- and D-isopulegol. A Perkin Elmer model 343 polarimeter with a cuvette length of 100 mm and a light source having a wavelength of 589 nm was utilized. All measurements took place at a constant temperature of 25° C. First, the enantiomer ratio of L- and D-isopulegol in % EE was determined by gas chromatography. Table 1 reports the measured values for the rotation values as a function of the EE (excess of L-isopulegol).

TABLE 1
Measured values for the rotation value measurements for
various enantiomer ratios of L- and D-isopulegol.
% EE valueOptical rotation [°]
12.56−0.82
30.84−4.522
58.8−10.42
90.6−17.77
97.88−19.66
99.84−20.17

FIG. 3 shows a graphical plot of the measured values from table 1. The measured values fit a 2nd order polynomial regression very well.

+ Open protocol
+ Expand
5

Comprehensive Structure Elucidation of Compound

Check if the same lab product or an alternative is used in the 5 most similar protocols
NMR spectra were obtained on a Bruker Avance 500 spectrometer at 25 °C (operating at 500 MHz for 1H-NMR, 125 MHz for 13C-NMR) with residual solvent peaks as references (CDCl3-d6: δH 7.26, δC 77.16). High-resolution electrospray ionization mass spectrometry (HR-ESIMS) measurements were obtained on an Accurate-Mass-Q-TOF LC/MS 6520 instrument (Santa Clara, CA, USA) in the positive ion mode. Optical rotations were measured on a Perkin-Elmer Model 343 polarimeter. Compound structures were elucidated by analyzing 1H NMR, 13C NMR, Heteronuclear Multiple Bond Correlation (HMBC), Heteronuclear Single Quantum Correlation (HSQC), 1H-1H Correlation Spectroscopy (COSY), and comparison with the previously reported data. The structure formula was finally confirmed by HR-ESIMS.
+ Open protocol
+ Expand
6

Analytical Characterization of Organic Compounds

Check if the same lab product or an alternative is used in the 5 most similar protocols
Optical rotations were measured with Perkin Elmer/Model-343 digital polarimeter. IR spectra were recorded on a JASCO FT/IR-480 spectrophotometer and reported as wave number (cm−1). 1H, 13C NMR spectra and 2D NMR spectra were recorded on a Bruker Avance III 600 spectrometer. Chemical shifts were reported using TMS as the internal standard. HR-ESI–MS data were obtained on a Bruker Apex IV FT-MS spectrometer. Column chromatography (CC) was carried out using D-101 macroreticular resin (Tianjin Polymer Technology Co. Ltd.), MCI gel (75–150 μm, Mitsubishi Chemical Industries, Japan) and silica gel (90–200 µm; Qingdao Marine Chemical Co. Ltd., Qingdao, People’s Republic of China). MPLC was performed on a Lisui EZ Purify III System packed with RP-18 silica gel (40–63 μm, Merck, 71 Darmstadt, Germany) columns. Precoated silica gel GF254 plates (Qingdao Marine Chemical Co. Ltd, Qingdao, People’s Republic of China) were used for thin-layer chromatography (TLC). Preparative HPLC was performed on Shimadzu LC-8A equipped with a Shimadzu PRC-ODS(K) column and Agilent 1100 apparatus equipped with a Zorbax SB-C-1875 (Agilent, 9.4 mm × 25 cm) column, respectively.
+ Open protocol
+ Expand
7

Spectroscopic Analysis of Natural Compounds

Check if the same lab product or an alternative is used in the 5 most similar protocols
Optical rotations were measured at 24 • C on a PerkinElmer Model 343 polarimeter. 1D and 2D NMR spectra were recorded in CD 3 OD, DMSO-d 6 and CDCl 3 in a Bruker 500 MHz NMR instrument (Avance 500). High-resolution mass spectra were obtained in a QTOF, Bruker Daltonics, model Impact II spectrometer in electrospray ionization. C18 columns (75 × 2.0 mm i.d.; 1.6 μm Shim-pack XR-ODS III) were used for UHPLC separation using a Shimadzu, model Nexera X2. Silica gel 60 (0.063-0.200 mm) and silica gel 60 (0.04-0.063 mm) were used for purification of the compounds. TLC was performed on normal phase precoated silica gel 60 G or 60 GF 254 (Merck) plates. The UV and ECD spectra of 1-3 were recorded with a Jasco J-815 spectrometer (Jasco, Tokyo, Japan) in the 195-400 nm region using the following parameters: bandwidth 1 nm; 25 response 1 s; scanning speed 100 nm min -1 ; 3 accumulations; room temperature; sample in methanol solution; 0.1 cm cell path length; concentration 0.2 mg mL -1 .
+ Open protocol
+ Expand

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

Sign up now

Revolutionizing how scientists
search and build protocols!