Chloroform
It is widely used as a solvent, anesthetic, and reagent in organic synthesis and chemical research.
Chloroform has a long history of medical and industrial applications, though its use has been restricted due to concerns over potential health hazards.
Researchers conducting chloroform-related experiments can optimize their workflows by leveraging the powerful comparison features of PubCompare.ai, an AI-driven tool that helps locate the most reliable and effecient protocols from the scientific literature, preprints, and patents.
This resource can enhance reproducibility and accuracy in chloroform-based studies, supporting the advancement of related fields.
Most cited protocols related to «Chloroform»
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Example 28
A typical protocol used for the synthesis of the PNAEP67-PnBA500 diblock copolymer was as follows: PNAEP67 macro-CTA (0.185 g, 14.6 μmol), deionised water (4.501 g, corresponding to a 20% w/w solution) and KPS (1.320 mg, 4.9 μmol; PNAEP67/KPS=3.0) were weighed into a 10 mL round-bottom flask charged with a magnetic flea. HCl (10 μL, 0.2 M) was added to reduce the pH to 3.0. This flask was then immersed in an ice bath, and the solution was degassed with nitrogen for 30 min. nBA (1.500 g) was weighed into a separate 14 mL vial and degassed with nitrogen in an ice bath for 30 min. An AsAc stock solution (0.01% w/w) was weighed into a second 14 mL vial and degassed with nitrogen in an ice bath for 30 min. After 30 min nBA (1.05 ml, 7.32 mmol; target DP=500) was added to the flask using a degassed syringe and needle under nitrogen. The flask contents were then stirred vigorously to ensure thorough mixing and degassed for 5 min before being immersed in an oil bath set at 30° C. After 1 min, AsAc (0.09 ml, 4.9 μmol; KPS/AscAc molar ratio=1.0) was added to the flask. The nBA polymerisation was allowed to proceed for 1 h before being quenched by exposing the reaction solution to air and immersing the reaction vial in an ice bath. 1H NMR spectroscopy analysis of the disappearance of vinyl signals indicated a final nBA conversion of 99%. Chloroform GPC analysis of this copolymer indicated a Mn of 86.6 kg mol−1 and an Mw/Mn of 1.56. Other diblock copolymer compositions were obtained by adjusting the nBA/PNAEP67 molar ratio.
Example 1
This example describes an exemplary nanostructure (i.e. nanocomposite tecton) and formation of a material using the nanostructure.
A nanocomposite tecton consists of a nanoparticle grafted with polymer chains that terminate in functional groups capable of supramolecular binding, where supramolecular interactions between polymers grafted to different particles enable programmable bonding that drives particle assembly (
Once synthesized, nanocomposite tectons were functionalized with either diaminopyridine-polystyrene or thymine-polystyrene were readily dispersed in common organic solvents such as tetrahydrofuran, chloroform, toluene, and N,N′-dimethylformamide with a typical plasmonic resonance extinction peak at 530-540 nm (
A key feature of the nanocomposite tectons is that the sizes of their particle and polymer components can be easily modified independent of the supramolecular binding group's molecular structure. However, because this assembly process is driven via the collective interaction of multiple diaminopyridine and thymine-terminated polymer chains, alterations that affect the absolute number and relative density of diaminopyridine or thymine groups on the nanocomposite tecton surface impact the net thermodynamic stability of the assemblies. In other words, while all constructs should be thermally reversible, the temperature range over which particle assembly and disassembly occurs should be affected by these variables. To better understand how differences in nanocomposite tecton composition impact the assembly process, nanostuctures were synthesized using different nanoparticle core diameters (10-40 nm) and polymer spacer molecular weights (3.7-11.0 kDa), and allowed to fully assemble at room temperature (˜22° C.) (
From these data, two clear trends can be observed. First, when holding polymer molecular weight constant, Tm increases with increasing particle size (
All nanocomposite tectons possess similar polymer grafting densities (i.e. equivalent areal density of polymer chains at the inorganic nanoparticle surface,
Conversely, for a fixed inorganic particle diameter (and thus constant number of polymer chains per particle), increasing polymer length decreases the areal density of diaminopyridine and thymine groups at the nanocomposite tecton periphery due to the “splaying” of polymers as they extend off of the particle surface, thereby decreasing Tm in a manner consistent with the trend in
Importantly, because the nanocomposite tecton assembly process is based on dynamic, reversible supramolecular binding, it should be possible to drive the system to an ordered equilibrium state where the maximum number of binding events can occur. The particle cores and polymer ligands are polydisperse (
To test this hypothesis, multiple sets of assembled nanocomposite tectons were thermally annealed at a temperature just below their Tm, allowing particles to reorganize via a series of binding and unbinding events until they reached the thermodynamically most stable conformation. The resulting structures were analyzed with small angle X-ray scattering, revealing the formation of highly ordered mesoscale structures where the nanoparticles were arranged in body-centered cubic superlattices (
Example 125
Methyl 4-((5-(benzyloxy)-2-methoxyphenyl)(ethyl)amino)butanoate (184). 5-(Benzyloxy)-N-ethyl-2-methoxyaniline (146) (0.681 g, 2.65 mmol), DIEA (0.92 mL, 5.3 mmol), and methyl 4-iodobutyrate (0.72 mL, 5.3 mmol) in DMF (5 mL) were stirred at 70° C. for 5 days. The reaction mixture was cooled to rt, diluted with EtOAc (60 mL), washed with water (4×50 mL), brine (75 mL), dried over Na2SO4 and evaporated. The residue was purified by chromatography on a silica gel column (2.5×30 cm bed, packed with CHCl3), eluant: 5% MeOH in CHCl3 to get compound 184 (0.72 g, 76%) as a dark amber oil.
Methyl 4-(ethyl(5-hydroxy-2-methoxyphenyl)amino)butanoate (186). Ester 184 (0.72 g, 2.0 mmol) was stirred under reflux with 6 mL of water and 6 mL of conc HCl for 1.5 hrs and then evaporated to dryness to give acid 185 as a brown gum. The crude acid was dissolved in 50 mL of methanol containing 1 drop (cat.) of methanesulfonic acid ant the solution was kept for 2 hrs at rt. After that the mixture was concentrated in vacuum and the residue was mixed with 20 mL of saturated NaHCO3. The product was extracted with EtOAc (3×40 mL). The extract was washed with brine (40 mL), dried over Na2SO4 and evaporated. The residue was purified by chromatography on a silica gel column (2.5×30 cm bed, packed with CHCl3), eluant: 5% MeOH in CHCl3 to get compound 186 (0.444 g, 83%) as a brown oil.
N-(6-(dimethylamino)-9-(4-(ethyl(4-methoxy-4-oxobutyl)amino)-2-hydroxy-5-methoxyphenyl)-3H-xanthen-3-ylidene)-N-methylmethanaminium chloride (187). To a stirred suspension of tetramethylrhodamine ketone 101 (0.234 g, 0.830 mmol) in 10 mL of dry chloroform was added oxalyl chloride (72 μL, 0.82 mmol) upon cooling to 0-5° C. The resulting red solution was stirred for 0.5 h at 5° C., and the solution of compound 186 (0.222 g, 0.831 mmol) in dry chloroform (5 mL) was introduced. The reaction was allowed to heat to rt, stirred for 72 h, diluted with CHCl3 (100 mL and washed with sat. NaHCO3 solution (2×30 mL) The organic layer was extracted with 5% HCl (3×25 mL). The combined acid extract was washed with CHCl3 (2×15 mL; discarded), saturated with sodium acetate and extracted with CHCl3 (5×30 mL). The extract was washed with brine (50 mL), dried over Na2SO4 and evaporated. The crude product was purified by chromatography on silica gel column (2×50 cm bed, packed with CHCl3/MeOH/AcOH/H2O (100:20:5:1)), eluant: CHCl3/MeOH/AcOH/H2O (100:20:5:1) to give the product 187 (0.138 g, 29%) as a purple solid.
4-((4-(6-(dimethylamino)-3-(dimethyliminio)-3H-xanthen-9-yl)-5-hydroxy-2-methoxyphenyl)(ethyl)amino)butanoate (188). Methyl ester 187 (0.136 g, 0.240 mmol) was dissolved in 5 mL of 1M KOH (5 mmol). The reaction mixture was kept at rt for 1.5 hrs and the acetic acid (1 mL) was added. The mixture was extracted with CHCl3 (4×30 mL), and combined extract was washed with brine (20 mL), filtered through the paper filter and. The crude product was purified by chromatography on silica gel column (2×50 cm bed, packed with MeCN/H2O (4:1)), eluant: MeCN/H2O/AcOH/(4:1:1) to give the product 188 (0.069 g, 98%) as a purple solid.
N-(6-(dimethylamino)-9-(4-((4-(2,5-dioxopyrrolidin-1-yloxy)-4-oxobutyl)(ethyl)amino)-2-hydroxy-5-methoxyphenyl)-3H-xanthen-3-ylidene)-N-methylmethanaminium chloride (189). To a solution of the acid 188 (69 mg, 0.12 mmol) in DMF (2 mL) and DIEA (58 μL, 0.33 mmol) was added N-hydroxysuccinimide trifluoroacetate (70 mg, 0.33 mmol). The reaction mixture was stirred for 30 min, diluted with chloroform (100 mL) and washed with water (5×50 mL), brine (50 mL), filtered through paper and concentrated in vacuum. The crude product was purified by precipitation from CHCl3 solution (5 mL) with ether (20 mL) to give compound 189 (55 mg, 67%) as a purple powder.
Example 35
2-(2,5-difluoro-4-(6-((6-(2,2,2-trifluoroethoxy)pyridin-3-yl)methoxy)pyridin-2-yl)benzyl)-1-(2-methoxyethyl)-1H-benzo[d]imidazole-6-carboxylic acid was prepared in a manner as described in Procedure 6. 1H NMR (400 MHz, Chloroform-d) δ 8.24 (d, J=19.5 Hz, 2H), 8.09 (d, J=8.5 Hz, 1H), 7.96 (d, J=8.4 Hz, 1H), 7.91-7.73 (m, 2H), 7.68 (t, J=8.0 Hz, 1H), 7.50 (d, J=7.5 Hz, 1H), 6.90 (d, J=8.4 Hz, 1H), 6.79 (d, J=8.2 Hz, 1H), 5.42 (s, 2H), 4.78 (dd, J=16.8, 8.5 Hz, 4H), 4.56 (s, 2H), 3.78 (d, J=5.2 Hz, 2H), 3.33 (s, 3H).
Example 122
To a stirred solution of crude 325 in MeCN (100 mL) under nitrogen at rt, was added dropwise a solution of 2,6-dimethylphenol (1.22 g, 10.0 mmol), triethylamine (4.18 mL, 30.0 mmol), and DABCO (0.112 g, 1.00 mmol) in MeCN over 30 min. The mixture immediately turned deep red at the beginning of addition, and was stirred an additional 90 min after addition was completed. The reaction mixture was concentrated by rotary evaporation, and the residue was redissolved in CHCl3 (300 mL). The solution was washed sequentially with sat. aq. NaHCO3 (1×300 mL) and brine (2×300 mL), dried over Na2SO4, filtered, and concentrated by rotary evaporation to give a crude red oil. Flash chromatography on the Combiflash (330 g column, 5 to 20% EtOAc in hexanes gradient), gave 326 (5.02 g, 85% yield over 2 steps) as an off-white solid foam.
1H NMR (400 MHz, CDCl3) δ 8.20 (d, J=7.4 Hz, 1H), 7.06 (s, 3H), 6.08 (d, J=7.4 Hz, 1H), 5.94 (d, J=15.9 Hz, 1H), 5.02 (dd, J=52.1 Hz, 3.1 Hz, 1H), 4.31 (d, J=13.8 Hz, 1H), 4.32-4.18 (m, 2H), 4.03 (dd, J=13.6 Hz, 2.0 Hz, 1H), 2.13 (s, 6H), 1.15-0.97 (m, 28H).
Top products related to «Chloroform»
More about "Chloroform"
This colorless, volatile, and non-flammable liquid has a distinctive sweet odor and has been used as a solvent, anesthetic, and reagent for many years.
Researchers working with chloroform can optimize their workflows by leveraging powerful comparison tools like PubCompare.ai.
This AI-driven platform helps scientists locate the most reliable and efficient protocols from the scientific literature, preprints, and patents, enhancing reproducibility and accuracy in chloroform-based studies.
In addition to chloroform, researchers may also work with related compounds such as TRIzol reagent and methanol.
TRIzol is a popular RNA extraction solution that utilizes the properties of chloroform, phenol, and guanidine isothiocyanate to isolate high-quality RNA from a variety of sample types.
The RNeasy Mini Kit is another widely used tool for RNA purification, while the NanoDrop spectrophotometer and Agilent 2100 Bioanalyzer are commonly employed for RNA quantification and quality assessment.
Reverse transcription, the process of converting RNA into complementary DNA (cDNA), is an essential step in many gene expression studies.
The High-Capacity cDNA Reverse Transcription Kit is a widely used tool for this purpose, allowing researchers to generate high-quality cDNA from their RNA samples.
By understanding the properties and applications of chloroform and related compounds, as well as leveraging the power of AI-driven tools like PubCompare.ai, researchers can optimize their workflows, enhance reproducibility, and drive advancements in their respective fields of study.