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Flash chromatography system

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The Flash Chromatography System is a laboratory instrument designed for the purification and separation of chemical compounds. It utilizes flash chromatography, a technique that employs pressurized solvent flow to efficiently separate and purify samples. The system allows for the rapid and effective separation of complex mixtures, making it a valuable tool for researchers and scientists working in various fields, such as organic synthesis, natural product isolation, and pharmaceutical development.

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Snap kp sil 750 g, by Biotage (2 mentions)

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Selekt flash chromatography system Isolera flash chromatography system FLASH column chromatography system SP1 Flash Chromatography Purification System Isolera One Flash Chromatography System

9 protocols using flash chromatography system

1

Deplete THC from Cannabis Oil

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Example 2

In this example, a Biotage Isolera Flash Chromatography System was employed to process raw cannabis oil to deplete THC component. In this example, a Biotage Isolera Flash Chromatography System was employed to process raw cannabis oil to deplete THC component. 45 g hemp oil (injection mass 6 wt %) was dissolved in 22.5 mL petroleum ether and injected to a 750 g normal phase silica gel column (SNAP KP-Sil 750 g, BIOTAGE) and rinsed with pet ether for a total injection volume of 67.5 mL. Solvent A was petroleum ether; Solvent B was 99.9% diethyl ether. Solvents A and B were employed to elute the column at 200 mL/min in a step gradient of 4 vol % B for 6 column volumes, then 8 vol % B for 4 column volumes, then 40 vol % B for 4 column volumes. Eluate was monitored at 220 nm and 240 nm. 120 mL fractions were collected. Following elution, the peak fractions were subjected to analytical HPLC or TLC analysis. Fractions 1-20 (1-6 CV) and 36-45 (11.5-14 CV) were combined and solvents removed by rotoevaporation. Analytical HPLC was employed to determine relative amounts of cannabinoids of interest.

US11084770B2. Cannabis extracts (2021-08-10). Treehouse Biotech, Inc. [US]. Inventors: Jacob Black [US], Ryan Beigie [US], Alex Mateo [US].
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2

Deplete THC from Cannabis Oil

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Example 2

In this example, a Biotage Isolera Flash Chromatography System was employed to process raw cannabis oil to deplete THC component. In this example, a Biotage Isolera Flash Chromatography System was employed to process raw cannabis oil to deplete THC component. 45 g hemp oil (injection mass 6 wt %) was dissolved in 22.5 mL petroleum ether and injected to a 750 g normal phase silica gel column (SNAP KP-Sil 750 g, BIOTAGE) and rinsed with pet ether for a total injection volume of 67.5 mL. Solvent A was petroleum ether; Solvent B was 99.9% diethyl ether. Solvents A and B were employed to elute the column at 200 mL/min in a step gradient of 4 vol % B for 6 column volumes, then 8 vol % B for 4 column volumes, then 40 vol % B for 4 column volumes. Eluate was monitored at 220 nm and 240 nm. 120 mL fractions were collected. Following elution, the peak fractions were subjected to analytical HPLC or TLC analysis. Fractions 1-20 (1-6 CV) and 36-45 (11.5-14 CV) were combined and solvents removed by rotoevaporation. Analytical HPLC was employed to determine relative amounts of cannabinoids of interest.

US10239808B1. Cannabis extracts (2019-03-26). Canopy Holdings, LLC [US]. Inventors: Jacob Black [US], Ryan Beigie [US], Alex Mateo [US].
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3

Alkylation of Triazole Derivatives

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The corresponding alkyl halide (2 eq.) was added in a sealed borosilicate tube containing triazole 9a (1 eq.) and sodium hydride (4 eq.) in anhydrous DMF (2 mL). The reaction was stirred at 45 °C for 60–90 minutes. When the end of reaction was determined by TLC (hexane: ethyl acetate 30%), mixture was diluted in 20 mL of ethyl acetate and washed with water (3 × 10 mL). The organic phase was dried over sodium sulphate, concentrated and purified by an isolation with FLASH Chromatography System (Biotage), using an ultra-10 g snap column (n-hexane: ethyl acetate, 10–50% gradient elution).
Santos S.N., Alves de Souza G., Pereira T.M., Franco D.P., de Nigris Del Cistia C., Sant'Anna C.M., Lacerda R.B, & Kümmerle A.E. (2019). Regioselective microwave synthesis and derivatization of 1,5-diaryl-3-amino-1,2,4-triazoles and a study of their cholinesterase inhibition properties. RSC Advances, 9(35), 20356-20369.
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4

Triazole Synthesis via Hydrazine Cyclization

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In a sealed borosilicate tube containing triazole (7a–7f) (1 eq.) in 2 mL of acetonitrile, it was added the corresponding hydrazine (1.1 eq.). Reaction was stirred at 100 °C for 40 minutes as shown in Table 3. After the end of the reaction, the reactional slurry was partitioned between ethyl acetate (20 mL) and water (10 mL). The organic phase was dried over anhydrous sodium sulphate and concentrated on a rotary evaporator. The products were separated with a FLASH Chromatography System (Biotage), using an ultra-10 g snap column (n-hexane: ethyl acetate, 5–75% gradient elution).
Santos S.N., Alves de Souza G., Pereira T.M., Franco D.P., de Nigris Del Cistia C., Sant'Anna C.M., Lacerda R.B, & Kümmerle A.E. (2019). Regioselective microwave synthesis and derivatization of 1,5-diaryl-3-amino-1,2,4-triazoles and a study of their cholinesterase inhibition properties. RSC Advances, 9(35), 20356-20369.
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5

Benzylpiperazine Triazole Synthesis

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Benzylpiperazine (3 eq.) was added in a sealed borosilicate tube containing triazole 10f–h (1 eq.) and acetonitrile (2 mL). Reaction was stirred at 60 °C until the end of the reaction, determined by TLC (DCM : methanol 10%). Then, mixture was concentrated and purified by an isolation with FLASH Chromatography System (Biotage), using an ultra-10 g snap column (DCM : methanol, 1–50% gradient elution).
Santos S.N., Alves de Souza G., Pereira T.M., Franco D.P., de Nigris Del Cistia C., Sant'Anna C.M., Lacerda R.B, & Kümmerle A.E. (2019). Regioselective microwave synthesis and derivatization of 1,5-diaryl-3-amino-1,2,4-triazoles and a study of their cholinesterase inhibition properties. RSC Advances, 9(35), 20356-20369.
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6

Synthesis of Pyrazolone Derivatives

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In a sealed borosilicate tube containing Boc-S-methyl-N-benzoyl-isothiourea intermediates 7a–d (1 eq.) in DMF (2 mL) it was added the corresponding hydrazine (1.1 eq.). The reaction was carried out in microwave irradiation at 150 °C for 60 minutes. After the end of the reaction, the slurry was partitioned between ethyl acetate (20 mL) and water (10 mL). The organic phase was dried over anhydrous sodium sulphate and concentrated on a rotary evaporator. Products were separated by FLASH Chromatography System (Biotage), using an ultra-10 g snap column (n-hexane: ethyl acetate, 5–75% gradient elution).
Santos S.N., Alves de Souza G., Pereira T.M., Franco D.P., de Nigris Del Cistia C., Sant'Anna C.M., Lacerda R.B, & Kümmerle A.E. (2019). Regioselective microwave synthesis and derivatization of 1,5-diaryl-3-amino-1,2,4-triazoles and a study of their cholinesterase inhibition properties. RSC Advances, 9(35), 20356-20369.
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7

Isolation of Mangiferin from Swertia chirata

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Mangiferin isolation was performed on a Biotage One Flash Chromatography system (Sweden), with UV detection and an automatic collector. For isolation of bio-active compound, the crude ethanolic extract (1 mg mL−1) prepared from the leaves of Swertia chirata by MAE was used. The Flash Chromatography conditions were as follows: 40 g flash column packed with 60–120 mesh sized silica gel; elution system: ethyl acetate/methanol gradient; wavelength: 254 and 280 nm and flow rate: 20 drop min−1. Before binding experiment, ethyl acetate was used to equilibrate the column former to isolation. Mangiferin was isolated in 40 min gradient program of solvent A (ethyl acetate) and solvent B (methanol). Out of seven fractions, mangiferin as the major peak was separated as first fraction (FA) after residue at wavelength 254 nm.
Structure of mangiferin compound in fractions was elucidated based on their spectral data (IR and 13C NMR). Purity of mangiferin compound was confirmed by comparison with reference compound (procured from Sigma Aldrich, USA) using HPTLC (high performance thin-layer chromatography) method.
Kaur P., Gupta R.C., Dey A., Malik T, & Pandey D.K. (2021). Optimization of harvest and extraction factors by full factorial design for the improved yield of C-glucosyl xanthone mangiferin from Swertia chirata. Scientific Reports, 11, 16346.
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8

Synthesis of Boc-Protected Lysine Derivative

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2 was synthesized by adapting
a previously reported method by Duspara et al.35 (link) H-Lys(Z)-OtBu·HCl (3.47 g, 9.34 mmol) was
dissolved in DMF (20 mL). DIPEA (1.63 mL, 9.34 mmol) was added to
the solution followed by 1 (3 g, 8.49 mmol, dissolved
in 10 mL DMF) dropwise and allowed to stir overnight at RT. The reaction
was diluted with EtOAc (100 mL) and washed with water (3 × 100
mL) and brine (3 × 100 mL). The organic layer was then dried
over magnesium sulfate, and the solvent was removed in vacuo. The crude product was purified using a Biotage Isolera flash chromatography
system (20–80% EtOAc/petroleum ether) to yield the desired
product as a colorless oil (4.5 g, 83%). 1H NMR (400 MHz,
chloroform-d) δ 7.38–7.30 (m, 5H), 5.22–5.02
(m, 5H), 4.33 (dd, J = 8.1, 4.9 Hz, 2H), 3.17 (dd, J = 6.4, 3.7 Hz, 2H), 2.28 (td, J = 9.6,
6.4 Hz, 2H), 1.44 (d, J = 1.1 Hz, 18H), 1.43 (s,
10H). 13C NMR (101 MHz, chloroform-d)
δ 172.41, 156.85, 156.59, 136.71, 128.46, 128.05, 128.00, 82.10,
81.75, 80.51, 77.33, 77.02, 76.70, 66.55, 53.29, 53.02, 40.65, 32.65,
31.60, 29.36, 28.36, 28.08, 28.03, 28.00, 22.24. ESI-MS: calc. for
[C32H51N3O9 + H]+ 622.36; found 622.3.
Rigby A., Firth G., Rivas C., Pham T., Kim J., Phanopoulos A., Wharton L., Ingham A., Li L., Ma M.T., Orvig C., Blower P.J., Terry S.Y, & Abbate V. (2022). Toward Bifunctional Chelators for Thallium-201 for Use in Nuclear Medicine. Bioconjugate Chemistry, 33(7), 1422-1436.
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9

Synthesis of Imidazole-Based Amino Acid Derivative

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1 was synthesized using a previously
reported method by Duspara et al.35 (link)l-Glutamic acid di-tert-butyl
hydrochloride (3.56 g, 12.04 mmol) and carbonyldiimidazole (2.15 g,
13.24 mmol) were dissolved in a 1:5 mixture of DMF/MeCN (50 mL) and
stirred at RT overnight. MeCN was then removed in vacuo, and the remaining DMF was diluted with EtOAc (100 mL) and washed
with water (3 × 50 mL) and brine (3 × 50 mL). The organic
layer was then dried over magnesium sulfate, and the solvent was removed in vacuo. The crude product was then purified using a Biotage
Isolera flash chromatography system (20–80% EtOAc/petroleum
ether) to yield the desired product as a colorless oil that solidified
upon standing (2.1 g, 51%). 1H NMR (400 MHz, chloroform-d) δ 8.16 (t, J = 1.1 Hz, 1H), 7.57
(d, J = 6.8 Hz, 1H), 7.41 (t, J =
1.5 Hz, 1H), 7.07 (dd, J = 1.6, 0.9 Hz, 1H), 2.48–2.38
(m, 2H), 2.27–2.05 (m, 2H), 1.47 (s, 9H), 1.43 (s, 9H). 13C NMR (101 MHz, chloroform-d) δ 174.00,
173.50, 173.34, 171.69, 162.78, 157.36, 149.11, 136.24, 135.17, 129.96,
121.71, 116.40, 77.43, 77.11, 76.79, 53.49, 52.72, 52.53, 52.38, 52.35,
52.12, 51.83, 51.78, 36.61, 31.51, 30.33, 30.07, 27.98, 27.94, 27.78,
26.15. ESI-MS: calc. for [C17H27N3O5 + H]+ 354.42; found 354.35.
Rigby A., Firth G., Rivas C., Pham T., Kim J., Phanopoulos A., Wharton L., Ingham A., Li L., Ma M.T., Orvig C., Blower P.J., Terry S.Y, & Abbate V. (2022). Toward Bifunctional Chelators for Thallium-201 for Use in Nuclear Medicine. Bioconjugate Chemistry, 33(7), 1422-1436.
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