Filtration
This technique is widely used in various industries, such as water treatment, pharmaceutical manufacturing, and chemical processing, to purify, concentrate, or isolate desired components.
Filtration can be achieved through a variety of methods, including mechanical, electrical, or chemical means, and the choice of filtration method depends on the specific application and the properties of the fluid and particles involved.
Effective filtration is crucial for ensuring product quality, enhancing process efficiency, and minimizing environmental impact.
Researchers and professionals in the field of filtration continually strive to optimize filtration processes through innovative technologies and techniques, such as the use of artificial intelligence and machine learning tools like PubCompare.ai, to enhance reproducibility, accuracy, and workflow efficiency.
Most cited protocols related to «Filtration»
Most recents protocols related to «Filtration»
Example 161
To a solution of 2-(piperazin-1-yl)ethanol (0.73 g, 5.6 mmol, 1 eq.) in DMF (10 mL) was added K2CO3 (1.56 g, 11.3 mmol, 2 eq.) followed by 1,2,4-trifluoro-5-nitrobenzene (1 g, 5.6 mmol, 1 eq.) and the mixture was stirred at 0° C. for 1 hour. The mixture was poured into ice-water (100 mL), extracted by EA (3×40 mL), and the organic layers were combined, washed with brine (150 mL), concentrated and purified via column chromatography (10-95% CH3CN—H2O) to afford 2-(4-(2,5-difluoro-4-nitrophenyl)piperazin-1-yl)ethanol (0.65 g, 41%) as a yellow solid.
To a solution of 2-(4-(2,5-difluoro-4-nitrophenyl)piperazin-1-yl)ethanol (0.65 g, 2.3 mmol) in MeOH (50 mL) was added Pd/C (100 mg) and the resulting mixture was stirred at r.t. overnight. The Pd/C was removed by filtration and the filtrate was concentrated to afford 2-(4-(4-amino-2,5-difluorophenyl)piperazin-1-yl)ethanol (0.58 g, 99%).
To a suspension of 2-(4-(4-amino-2,5-difluorophenyl)piperazin-1-yl)ethanol (270 mg, 0.88 mmol, 1 eq.) and N-(3-(2-chloroquinazolin-8-yl)phenyl)acrylamide (225 mg, 0.88 mmol, 1 eq.) in n-BuOH (10 mL) was added TFA (0.5 mL, 4.4 mmol, 5 eq.) and the resulting mixture was stirred at 90° C. overnight. The mixture was concentrated, diluted with DCM (20 mL), washed with Na2CO3 solution (20 mL), dried, concentrated and purified via column chromatography (DCM/MeOH=10/1) to afford N-(3-(2-((2,5-difluoro-4-(4-(2-hydroxyethyl)piperazin-1-yl)phenyl)amino)quinazolin-8-yl)phenyl)acrylamide (120 mg, 26%) as yellow solid. LRMS (M+H+) m/z calculated 531.2, found 531.2. 1H NMR (DMSO-d6, 400 MHz) δ 10.18 (s, 1H), 9.37 (s, 1H), 9.17 (s, 1H), 7.97-7.94 (m, 3H), 7.83-7.74 (m, 2H), 7.50-7.39 (m, 3H), 6.90-6.85 (m, 1H), 6.48-6.41 (m, 1H), 6.23 (dd, 1H), 5.73 (dd, 1H), 4.42 (t, 1H), 3.55-3.50 (m, 2H), 2.94-2.91 (m, 4H), 2.55-2.54 (m, 4H), 2.44 (t, 2H).
Example 26
Synthesis of 169-A.
A mixture of tert-butyl hexahydropyrrolo[3,4-c]pyrrole-2(1H)-carboxylate (750 mg, 3.54 mmol), 1-methylpiperidin-4-one (800 mg, 7.08 mmol) and acetic acid (2 drops) in DCE (15 mL) was stirred at 50° C. for 2 h. Then Sodium triacetoxyborohydride (1.50 g, 7.08 mmol) was added into above mixture and stirred at 50° C. for another 2 h. After the reaction was completed according to LCMS, the solvent was diluted with water (10 mL) and then extracted by DCM (10 mL×3). The combined organics washed with brine (10 mL×3), dried over anhydrous Na2SO4 and then concentrated in vacuo. The residue was purified by column chromatography on silica gel (DCM:MeOH=100:1˜50:1) to give 169-A (750 mg, 69%) as a yellow oil.
Synthesis of 169-B.
A solution of 169-A (400 mg, 1.29 mmol) in DCM (10 mL) was added TFA (5 mL) and stirred at room temperature for 1 h. when LCMS showed the reaction was finished. The solvent was removed in vacuo to give 169-B as a crude product and used to next step directly.
Synthesis of 169-C.
A mixture of 143-C (306 mg, 0.65 mmol) and 169-B (crude product from last step) in acetonitrile (6 mL) was stirred at 50° C. for 30 min. Then Na2CO3 (624 mg, 6.50 mmol) was added into above mixture and stirred at 50° C. for 3 h. After the reaction was completed according to LCMS, the mixture was cooled to room temperature. The Na2CO3 was removed by filtered. The filtrate was concentrated in vacuo. The residue was purified by column chromatography on silica gel (DCM:MeOH=100:1˜20:1) to give 169-C (230 mg, 76%) as a yellow solid.
Synthesis of 169.
A mixture of 169-C (230 mg, 0.49 mmol) and Pd/C (230 mg) in MeOH (10 mL) was stirred at room temperature for 30 min under H2 atmosphere. Pd/C was then removed by filtration through the Celite. The filtrate was concentrated and the residue was purified by Pre-TLC (DCM:MeOH=10:1) to give 169 (150 mg, 70%) as a white solid.
Compounds 152, 182, 199, 201, 202, 203, 235, 236 and 256 were synthesized in a similar manner using the appropriately substituted aldehyde or ketone variant of 169.
Compound 152.
50 mg, 36%, a light yellow solid.
Compound 182.
70 mg, 38%, a red solid.
Compound 199.
50 mg, 54%, a light yellow solid.
Compound 201.
30 mg, 42%, as a yellow solid.
Compound 202.
30 mg, 42%, a yellow solid.
Compound 203.
30 mg, 18%, a yellow solid.
Compound 235.
170 mg, 87%, a white solid.
Compound 236.
70 mg, 50%, a white solid.
Compound 256.
20 mg, 8%, a light yellow solid.
Compounds 210, 211, 215, 222, 223, 242 and 262 were synthesized in a similar manner using the appropriately substituted amine variant of 169.
Compound 210.
160 mg, 96%, a tan solid.
Compound 211.
70 mg, 40%, a white solid
Compound 215.
70 mg, 75%, a white solid.
Compound 222.
30 mg, 42%, a yellow solid.
Compound 223.
35 mg, 31%, a white solid.
Compound 242.
50 mg, 34%, a white solid.
Compound 262.
38 mg, 43%, a white solid.
Example 1
InCl (1 eq.) was added to a Schlenk flask charged with LiCp(CH2)3NMe2 (11 mmol) in Et2O (50 mL). The reaction mixture was stirred overnight at room temperature. After filtration of the reaction mixture, the solvent was evaporated under reduced pressure to obtain a red oil. After distillation a yellow liquid final product was collected (mp˜5° C.). Various measurements were done to the final product. 1H NMR (C6D6, 400 MHz): δ 5.94 (t, 2H, Cp-H), 5.82 (t, 2H, Cp-H), 2.52 (t, 2H, N—CH2—), 2.21 (t, 2H, Cp-CH2—), 2.09 (s, 6H, N(CH3)2, 1.68 (q, 2H, C—CH2—C). Thermogravimetric (TG) measurement was carried out under the following measurement conditions: sample weight: 22.35 mg, atmosphere: N2 at 1 atm, and rate of temperature increase: 10.0° C./min. 97.2% of the compound mass had evaporated up to 250° C. (Residue <2.8%). T (50%)=208° C. Vacuum TG measurement was carried out under delivery conditions, under the following measurement conditions: sample weight: 5.46 mg, atmosphere: N2 at 20 mbar, and rate of temperature increase: 10.0° C./min. TG measurement was carried out under delivery conditions into the reactor (about 20 mbar). 50% of the sample mass is evaporated at 111° C.
Using In(Cp(CH2)3NMe2) synthesized in Example 1 as an indium precursor and H2O and O3 as reaction gases, indium oxide film may be formed on a substrate by ALD method under the following deposition conditions. First step, a cylinder filled with In(Cp(CH2)3NMe2) is heated to 90° C., bubbled with 100 sccm of N2 gas and the In(Cp(CH2)3NMe2) is introduced into a reaction chamber (pulse A). Next step, O3 generated by an ozone generator is supplied with 50 sccm of N2 gas and introduced into the reaction chamber (pulse B). Following each step, a 4 second purge step using 200 sccm of N2 as a purge gas was performed to the reaction chamber. 200 cycles were performed on a Si substrate having a substrate temperature of 150° C. in the reaction chamber at a pressure of about 1 torr. As a result, an indium oxide film will be obtained at approximately 150° C.
Example 2
Same procedure as Example 1 started from Li(CpPiPr2) was performed to synthesize In(CpPiPr2). An orange liquid was obtained. 1H NMR (C6D6, 400 MHz): δ 6.17 (t, 2H, Cp-H), 5.99 (t, 2H, Cp-H), 1.91 (sept, 2H, P—CH—), 1.20-1.00 (m, 12H, C—CH3).
Using In(CpPiPr2) synthesized in Example 2 as the indium precursor and H2O and O3 as the reaction gases, indium oxide film may be formed on a substrate by the ALD method under the following deposition conditions. First step, a cylinder filled with In(CpPiPr2) is heated to 90° C., bubbled with 100 sccm of N2 gas and the In(CpPiPr2) is introduced into a reaction chamber (pulse A). Next step, O3 generated by an ozone generator is supplied with 50 sccm of N2 gas and introduced into the reaction chamber (pulse B). Following each step, a 4 second purge step using 200 sccm of N2 as a purge gas was performed to the reaction chamber. 200 cycles were performed on the Si substrate having a substrate temperature of 150° C. in an ALD chamber at a pressure of about 1 torr. As a result, an indium oxide was obtained at 150° C.
Example 1
10 g (33.09 mmol) of 1-(2-fluoro-6-trifluoromethyl-benzyl)-6-methyl-1H-pyrimidine-2,4-dione (III), 6.8 g (49.62 mmol) of K2CO3 and 2.4 g (6.6 mmol) of tetrabutylammonium iodide were mixed with 50 mL of acetone at the temperature of about 20° C. Subsequently, 13.6 g (43.12 mmol) of (R)-2-((tert-butoxycarbonyl)amino)-2-phenylethyl methanesulfonate (IVa) were added and the obtained mixture was heated at the temperature of about 55° C. and maintained under stirring for about 16 hours at said temperature.
Once this maintenance was finished, the solvent was vacuum distilled and 50 mL of ethyl acetate and 50 mL of water were added to the residue thus obtained. A 1 M aqueous solution of HCl was slowly added, maintaining the temperature between 20 and 25° C. until achieving a pH of between 7 and 8. The aqueous phase was separated and treated with 3 fractions of 30 mL each of ethyl acetate. All the organic extracts were pooled and the solvent was removed by means of vacuum to obtain a slightly yellowish oily residue to which 45 mL of methanol were added, obtaining complete dissolution of the residue.
Example 2
16.1 g (99.24 mmol) of iodine monochloride (ICI) were dissolved in 40 mL of methanol at the temperature of about 10° C. The methanol solution previously obtained according to the methodology described in Example 1 comprising 3-((R)-2-(tert-butoxycarbonyl)amino-2-phenylethyl)-1-(2-fluoro-6-trifluoromethylbenzyl)-6-methyl-1H-pyrimidine-2,4-dione (II) was added to the iodine monochloride solution, maintaining the temperature between 20 and 25° C. Once the addition was finished, the obtained solution was heated to about 50° C. and was maintained under stirring for 2 hours at the mentioned temperature.
Once the maintenance was finished, the solvent was vacuum distilled and 50 mL of acetone were slowly added to the obtained oily residue at the temperature of between and 25° C. The addition of acetone caused a solid precipitate to appear almost immediately. The obtained mixture was maintained for 1 hour under stirring at the mentioned temperature. The resulting solid was isolated by filtration, washed with two fractions of 25 mL of acetone, and finally dried at the temperature of 50° C. to obtain 15.6 g (80.8% yield) of a white solid corresponding to the 3-((R)-2-(amino-2-phenylethyl)-1-(2-fluoro-6-trifluoromethylbenzyl)-5-iodo-6-methyl-1H-pyrimidine-2,4-dione hydrochloride salt (Ia) (UHPLC purity: 98.9%).
1H-NMR (d6-DMSO, 400 MHz) δ (ppm): 8.70 (2H, s broad), 7.65-7.48 (3H, m), 7.40-7.32 (5H, m), 5.40-5.29 (2H, dd), 4.47 (1H, t), 4.25 (2H, dd), 2.65 (3H, s).
13C-NMR (d6-DMSO, 100 MHz) δ (ppm): 161.87, 159.47, 159.41, 154.19, 150.98, 134.70, 129.93, 129.84, 129.01, 128.58, 127.38, 122.61, 122.34, 122.22, 121.34, 121.10, 74.80, 52.26, 45.45, 44.60, 25.66.
The DSC of this compound is shown in
Example 17
50 μmol (Gd3+) of AGuIX® were redispersed in 125 μl of ultrapure water in order to obtain a solution at 400 mM [Gd3+]. 2.8 mg of cisplatin are placed in a 2.5 ml flask. 1.1 ml of ultrapure water are added to the flask, which is stirred. Since cisplatin is not very soluble at ambient temperature, it is necessary to heat to 40° C. until it is completely dissolved. A solution containing 2.5 g/l of cisplatin is then obtained, and is protected from the light with aluminium. 229 μl of this solution are then added to the solution of AGuIX®, as are 146 μl of ultrapure water. The flask is stirred for 30 minutes in the dark. A solution containing 100 mM of gadolinium and 1160 mg/l of cisplatin is thus obtained.
This solution is placed in a 3 kDa Vivaspin®, and a tangential filtration cycle is carried out so as to obtain a supernatant of 160 μl. The subnatant is analysed by UV-visible analysis. The cisplatin is detectable by UV/VIS absorption at a wavelength of 706 nm after reaction with ODPA. For the reaction with cisplatin, a solution of ODPA at 1.4 mg/ml and a phosphate buffer (pH 6.8) are prepared. The subnatant is diluted 5-fold. 140 μl of this solution are added to 200 μl of buffer and 100 μl of ODPA. The resulting solution is heated at 100° C. for 15 min.
Once the reaction is finished and the temperature has returned to ambient temperature, 560 μl of DMF are added. The final solution is filtered and then analysed by UV-visible analysis.
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More about "Filtration"
This technique is widely employed in various industries, including water treatment, pharmaceutical manufacturing, and chemical processing, to purify, concentrate, or isolate desired components.
The filtration process can be achieved through a variety of methods, such as mechanical, electrical, or chemical means, and the choice of filtration method depends on the specific application and the properties of the fluid and particles involved.
Effective filtration is crucial for ensuring product quality, enhancing process efficiency, and minimizing environmental impact.
Researchers and professionals in the field of filtration continually strive to optimize filtration processes through innovative technologies and techniques, such as the use of artificial intelligence and machine learning tools like PubCompare.ai, to enhance reproducibility, accuracy, and workflow efficiency.
Filtration can be used to separate a wide range of materials, including Whatman No. 1 filter paper, fetal bovine serum (FBS), penicillin/streptomycin, Whatman filter paper, Dulbecco's Modified Eagle Medium (DMEM), No. 1 filter paper, dimethyl sulfoxide (DMSO), deoxyribonuclease I (DNase I), and bovine serum albumin (BSA).
The choice of filtration method and materials will depend on the specific application and the properties of the fluid and particles involved.
For example, Whatman No. 1 filter paper is commonly used for general filtration purposes, while FBS and penicillin/streptomycin may be used in cell culture applications.
DMEM and DMSO are also commonly used in cell culture and related research.
Researchers may also use DNase I and BSA in various filtration and purification processes.
The use of AI-powered tools like PubCompare.ai can help optimize filtration research by enabling researchers to compare and identify the best filtration protocols from the literature, preprints, and patents, enhancing reproducibility, accuracy, and workflow efficiency.
This can be particularly useful in streamlining filtration projects and ensuring the highest quality results.