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Autopure

Manufactured by Waters Corporation

The Autopure is a laboratory instrument designed for automated DNA and RNA purification. It utilizes a combination of magnetic bead and column-based technology to efficiently extract and purify nucleic acids from a variety of sample types. The Autopure is capable of processing multiple samples simultaneously, providing a streamlined and standardized purification workflow to support various research applications.

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6 protocols using autopure

1

Characterization of Organic Compounds

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Example 1

Unless otherwise stated, all commercially available materials were purchased from Bachem, Aldrich, P3 BioSystems, or other vendors and were used as received. All non-aqueous reactions were performed under argon in oven-dried glassware. Routine monitoring of reactions was performed using Waters Acquity Ultra Performance Liquid Chromatography (UPLC). All HPLC purifications were done by Varian PrepStar HPLC system or Waters Autopure (mass directed purification system) using Prep C18 5 μm OBD (19×150 mm) column. 1H- and 13C-NMR spectra were acquired on a Bruker DRX-500 spectrometer. Chemical shifts 6 are expressed in parts per million, with the solvent resonance as an internal standard (chloroform-d, 1H: 7.26; 13C: 77.16 ppm; DMSO-d6, 1H: 2.50 ppm; 13C: 39.52 ppm). Hexafluorobenzene was used as internal standard for 19F NMR. NMR data are reported as following: chemical shift, multiplicity (s=singlet, d=doublet, t=triplet, q=quartet, m=multiplet, br=broad), coupling constant, and integration.

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2

Characterization of Organic Compounds

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Example 1

Unless otherwise stated, all commercially available materials were purchased from Bachem, Aldrich, P3 BioSystems, or other vendors and were used as received. All non-aqueous reactions were performed under argon in oven-dried glassware. Routine monitoring of reactions was performed using Waters Acquity Ultra Performance Liquid Chromatography (UPLC). All HPLC purifications were done by Varian PrepStar HPLC system or Waters Autopure (mass directed purification system) using Prep C18 5 μm OBD (19×150 mm) column. 1H- and 13C-NMR spectra were acquired on a Bruker DRX-500 spectrometer. Chemical shifts 6 are expressed in parts per million, with the solvent resonance as an internal standard (chloroform-d, 1H: 7.26; 13C: 77.16 ppm; DMSO-d6, 1H: 2.50 ppm; 13C: 39.52 ppm). Hexafluorobenzene was used as internal standard for 19F NMR. NMR data are reported as following: chemical shift, multiplicity (s=singlet, d=doublet, t=triplet, q=quartet, m=multiplet, br=broad), coupling constant, and integration.

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3

Synthesis of Diverse Amide Compounds

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All commercially available materials were purchased from Bachem, Aldrich, P3 BioSystems, or other vendors and were used as received unless stated otherwise. All non-aqueous reactions were performed under argon in oven-dried glasswares. Reactions were monitored using Waters Acquity Ultra Performance Liquid Chromatography (UPLC). All HPLC purifications were done by Varian PrepStar HPLC system or Waters Autopure (mass directed purification system) using Prep C18 5μm OBD (19 X 150 mm) column. 1H- and 13C- NMR spectra were acquired on a Bruker DRX-500 spectrometer. Chemical shifts δ are expressed in parts per million, with the solvent resonance as an internal standard (chloroform-d, 1H: 7.26; 13C: 77.16 ppm; DMSO-d6, 1H: 2.50 ppm; 13C: 39.52 ppm). Hexafluorobenzene was used as internal standard for 19F NMR. NMR data are reported as following: chemical shift, multiplicity (s = singlet, d = doublet, t = triplet, q = quartet, m = multiplet, b = broad), coupling constant, and integration. We followed our reported procedure for HATU or EDC mediated amide bond formation, boc-deprotection and O-debenzylation.37 (link),38 (link) All final compounds are > 95% pure.
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4

NMR Spectroscopy and UPLC/MS Characterization

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1H- and 13C- NMR spectra were acquired on a Bruker DRX-500 spectrometer. Chemical shift δ is expressed in parts per million, with the solvent resonance as an internal standard (CDCl3, 1H: 7.26; 13C: 77.16 ppm; DMSO-d6, 1H: 2.50 ppm; 13C: 39.52 ppm). NMR data are reported as follows: chemical shift, multiplicity (br = broad, d = doublet, q = quartet, m = multiplet, s = singlet, t = triplet), coupling constant, and integration. All reactions in aprotic solvents were performed under argon in oven-dried glassware. Reaction progress was monitored on a Waters Acquity Ultra Performance Liquid Chromatography (UPLC/MS). All HPLC purifications were performed on a Waters Autopure (mass directed purification system) equipped with a Prep C18 5μm OBD (19 × 150 mm) column. High Resolution Mass Spectra (HRMS) of final products were collected on a PE SCIEX API 100. Unless otherwise stated, all commercially available materials were purchased from Aldrich, P3 BioSystems, Combi-Blocks or other vendors and were used as received. The purity of all final compounds were > 95% as determined on a Waters Acquity Ultra Performance Liquid Chromatography (UPLC/MS) using the following method: gradient (5–95% ACN + 0.1% formic acid in water + 0.1% formic acid over 7.5 min, followed by 95% ACN + 0.1% formic acid for 0.5 min); flow rate 0.3 mL/min, column ACQUITY UPLC® BEH C18 1.7μM (2.1 × 50mm).
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5

Synthesis of Small Molecules via UPLC/MS

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Unless otherwise stated, all commercially available materials were purchased from Aldrich, P3 BioSystems, Combi-Blocks or other vendors and were used as received. All reactions in aprotic solvents were performed under argon in oven-dried glassware. Reaction progress was monitored on a Waters Acquity Ultra Performance Liquid Chromatography (UPLC/MS). All HPLC purifications were performed on a Waters Autopure (mass directed purification system) equipped with a Prep C18 5μm OBD (19 × 150 mm) column. 1H- and 13C-NMR spectra were acquired on a Bruker DRX-500 spectrometer. Chemical shift δ is expressed in parts per million, with the solvent resonance as an internal standard (CDCl3, 1H: 7.26; 13C: 77.16 ppm; DMSO-d6, 1H: 2.50 ppm; 13C: 39.52 ppm). NMR data are reported as follows: chemical shift, multiplicity (br = broad, d = doublet, q = quartet, m = multiplet, s = singlet, t = triplet), coupling constant, and integration. High Resolution Mass Spectra (HRMS) of final products were collected on a PE SCIEX API 100.
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6

Standard Materials and Characterization Methods

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Example 1

Unless otherwise stated, all commercially available materials were purchased from Bachem, Aldrich, P3 BioSystems, or other vendors and were used as received. All non-aqueous reactions were performed under argon in oven-dried glassware. Routine monitoring of reactions was performed using Waters Acquity Ultra Performance Liquid Chromatography (UPLC). All HPLC purifications were done by Varian PrepStar HPLC system or Waters Autopure (mass directed purification system) using Prep C18 5 μm OBD (19×150 mm) column. 1H- and 13C-NMR spectra were acquired on a Bruker DRX-500 spectrometer. Chemical shifts 6 are expressed in parts per million, with the solvent resonance as an internal standard (chloroform-d, 1H: 7.26; 13C: 77.16 ppm; DMSO-d6, 1H: 2.50 ppm; 13C: 39.52 ppm). Hexafluorobenzene was used as internal standard for 19F NMR. NMR data are reported as following: chemical shift, multiplicity (s=singlet, d=doublet, t=triplet, q=quartet, m=multiplet, br=broad), coupling constant, and integration.

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