Month: May 2021

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 4387-36-4, name is 2-Iodobenzonitrile, A new synthetic method of this compound is introduced below., name: 2-Iodobenzonitrile

S1:100 mmol of the compound of the above formula (1), 150 mmol of the compound of the above formula (2), 0.8 mmol of palladium acetate, 100 mmol of tetra-n-butylammonium bromide were added to an appropriate amount of the organic solvent N,N-dimethylacetamide (DMA) at room temperature. And 225 mmol of sodium carbonate, and then the temperature was raised to 95 ° C with stirring, and the reaction was stirred at this temperature for 25 hours;After the reaction was completed, the reaction mixture was poured into a sufficient amount of ethyl acetate, and then washed with saturated brine, and the organic layer and aqueous layer were separated, and the aqueous layer was extracted with ethyl acetate. The organic layer and the organic layer obtained by ethyl acetate extraction were dried over anhydrous Na 2 SO 4 and evaporated under reduced pressure. The elution is carried out, the eluent is collected and the eluent is removed by evaporation.The compound of the above formula (3) is thus a white solid, the yield is 87.6percent;

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Electric Literature of 16932-44-8, Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 16932-44-8, name is 2-Iodo-1,3-dimethoxybenzene, This compound has unique chemical properties. The synthetic route is as follows.

A mixture of 2,6-dimethoxyiodobenzene (40.1 mg, 151 mumol), Bu3SnH (48.7 muL, 181 mumol), and V-65 (7.5 mg, 30.2 mumol) in THF-d8 (4 mL) was stirred at reflux for 3 h. Bu3SnH (48.7 muL, 181 mumol) and V-65 (7.5 mg, 30.2 mumol) were added, and the mixture was stirred at reflux for 2 h. The mixture was concentrated in vacuo, and the residue was purified by column chromatography on silica gel (pentane/Et2O=40:1) to give 2-deutero-1,3-dimethoxybenzene (21.1 mg, 100%). 1H NMR (400 MHz): 3.72 (s, 6H, O-CH3), 6.46-6.51 (m, 2.15H, 2-H, 4-H, 6-H), 7.17 (t, J=8.1 Hz, 1H, 5-H); 2H NMR: 6.50 (br); MS(EI+): m/z 139 [M]+; HRMS (EI+): calcd for C8H92HO2 [M]+: 139.07436, found: 139.07515.

The chemical industry reduces the impact on the environment during synthesis 2-Iodo-1,3-dimethoxybenzene. I believe this compound will play a more active role in future production and life.

Electric Literature of 10297-05-9,Some common heterocyclic compound, 10297-05-9, name is 1-Chloro-4-iodobutane, molecular formula is C4H8ClI, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

4-Chloro-1-(3-pyridyloxy)butane Under a nitrogen atmosphere, a solution of 3-hydroxypyridine (3.50 g, 36.8 mmol) in N,N-dimethylformamide (DMF) (10 mL) was added drop-wise over 5 min to a cold (0-5° C.), stirring slurry of sodium hydride (1.16 g of an 80percent dispersion in mineral oil, 38.6 mmol) in DMF (40 mL). The mixture was allowed to stir and warm to ambient temperature over 1 h. The mixture was then cooled to 0-5° C., and 1-chloro-4-iodobutane (9.67 g, 44.2 mmol) was added drop-wise over 5 min. The resulting dark-brown mixture was stirred at ambient temperature for 2 h. Water (25 mL) was added, followed by saturated NaCl solution (25 mL), and the mixture was extracted with ether (4*50 mL). The combined ether extracts were dried (Na2SO4), filtered, and concentrated by rotary evaporation to a residue that was dried briefly under high vacuum to give 6.89 g (quantitative yield) of an oil.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-Chloro-4-iodobutane, its application will become more common.

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 620-05-3, name is (Iodomethyl)benzene, A new synthetic method of this compound is introduced below., Recommanded Product: (Iodomethyl)benzene

General procedure: In a flame-dried round-bottom flask, beta-amidoester (9) (1 mmol; 1 equiv) was taken in DMF (5 mL) at room temperature. To this reaction mixture KOt-Bu (1.2 mmol; 1.2 equiv) was added. After 5 minutes of stirring at same temperature alkyl halide (1.05 mmol; 1.05 equiv) was added and stirring was continued for 15 minutes. Upon completion of the alkylation (judged by TLC), it was diluted with 10 mL of EtOAc and quenched with water. The organic extracts were dried over anhydrous sodium sulphate and concentrated under vacuum. The crude product was purified by flash chromatography (hexane and EtOAc as eluents) to afford compounds 10.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Adding a certain compound to certain chemical reactions, such as: 3268-21-1, name is 1,4-Diiodo-2,3,5,6-tetramethylbenzene, belongs to iodides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 3268-21-1, Safety of 1,4-Diiodo-2,3,5,6-tetramethylbenzene

To a solution of 1 (3.02 g, 7.82 mmol, 1 equiv), Pd(PPh3)2Cl2 (0.380 g, 0.541 mmol, 0.07 equiv) and CuI (0.101 g, 0.530 mmol, 0.07 equiv) in Et2NH was added ethynyltrimethylsilane (2.45 mL, 17.3 mmol, 2.2 equiv) and the reaction was stirred at RT overnight. The solvent was evaporated followed by extraction with CH2Cl2 (3 >< 100 mL) and washing of the organic layer with H20 (2 >< 200 mL) and brine (250 mL). The combined organic layers were dried over MgSO4 and concentrated in vacuo. The product was (0279) purified via column chromatography (PE) leading to 2 as off-white crystals (82%). 1H NMR (400 MHZ, CDClg) 6 2.38 (s, 12H), 0.27 (s, 18H). 13C NMR (400 MHZ, CDC13)8 136.0, 123.4, 104.2, 103.2, 18.5, 0.27. IRV 2957, 2138, 1270, 1073, 863 cm-1. HRMS (EI+) m/z caIcuIated for C20H30Si2 326.1886, found 326.1870. If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Adding a certain compound to certain chemical reactions, such as: 2043-57-4, name is 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-8-iodooctane, belongs to iodides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 2043-57-4, Quality Control of 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-8-iodooctane

1-Methylimidazole (4.32 g, 0.52 mol) was partially dissolved in reagent-grade toluene (50 ml) in a large round-bottomed flask and stirred vigorously. 1, 1, 1,2,2,3,3,4,4,5,5, 6, 6-Tridecafluoro-8-iodooctane (26 g, 0.053 mol) was added, and the mixture was heated under reflux at 110 degrees C for 24 hours. The solvent was removed under vacuum giving l-methyl-3- (3, 3, 4, 4, 5, 5, 6, 6, 7, 7, 8, 8, 8 -tridecafluorooctyl) imidazolium iodide (30.5 g) as a waxy solid. Potassium 1,1,2,2- tetrafluoroethanesulfonate (TFES-K, 12 g) was added to reagent grade acetone (100 ml) in a separate round-bottomed flask, and this solution was carefully added to the 1- methyl-3- (3, 3, 4, 4, 5, 5, 6, 6, 7, 7, 8,8,8- tridecafluorooctyl) imidazolium iodide which had been dissolved in acetone (50 ml) . The reaction mixture was heated under reflux for approximately 16 hours. The reaction mixture was then filtered using a large frit glass funnel to remove the white KI precipitate formed, and the filtrate was placed on a rotary evaporator for 4 hours to remove the acetone. The oily liquid was then filtered a second time to yield the product, as shown by proton NMR.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-8-iodooctane, and friends who are interested can also refer to it.

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 27913-58-2, name is 4-(4-Iodophenyl)butanoic acid, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of 4-(4-Iodophenyl)butanoic acid

A solution of BORANE-TETRAHYDROFURAN (200M .) was added dropwise to a stirred solution of 4- (4-IODOPHENYL) butanoic acid (25g) at 0C under nitrogen. After 2h methanol (200MI) was added dropwise. And then the solvent was removed in vacuo. The residue was partitioned between ether and water and the organic phase was separated. The combined organic layers were dried (NA2SO4) and evaporated to give the title compound (23 g). LCMS RT = 3.34 min.

According to the analysis of related databases, 27913-58-2, the application of this compound in the production field has become more and more popular.

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 375-80-4, name is 1,6-Diiodoperfluorohexane belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. HPLC of Formula: C6F12I2

75 mg of a commercial mixture of alpha,omega-diiodoperfluorinated compounds (sold by Apollo Scientific Ltd.) composed of 25% tetrafluoro-1,2-diiodoethane (m=1), 25% octafluoro-1,4-tetraiodobutane (m=2), 25% dodecafluoro-1,6-diiodohexane (m=3) and 25% hexadecafluoro-1,8-diiodooctane (m=4) were solubilized in 1 ml of CHCl3, and separately 20 mg of sequestering agent of formula (CH3)3N+-(CH2)12-N+(CH3)3.2I-, i.e. dodecamethonium iodide, were solubilized in 1 ml of CH3OH.The two solutions were then mixed in a test tube which was then closed. After about 2 hours, the formation of a solid white precipitate was observed, which was filtered, washed twice with CCl4 and dried under vacuum. The results of the performed tests, as reported below, confirmed that this was an adduct of dodecamethonium iodide and dodecafluoro-1,6-diiodohexane.The dodecafluoro-1,6-diiodohexane was then separated from the sequestering agent by sublimation of the crystalline adduct under vacuum at a temperature of about 50 C. and recovered by recondensation at a temperature of about -198 C.100% pure dodecafluoro-1,6-diiodohexane was then obtained.The following tests were conducted on the crystalline adduct:melting point: 226 C.;IR (cm-1, selective bands): pure dodecamethonium iodide: 3002, 2914, 2851, 1483, 1464, 973, 939, 916, 731; adduct of dodecamethonium iodide and dodecafluoro-1,6-diiodohexane: 3010, 2941, 2867, 1475, 1203, 1141, 1125, 1081, 963, 909, 731. 19F NMR (470.6 MHz, CD3OD, 0.002 M): adduct of dodecamethonium iodide and dodecafluoro-1,6-diiodohexane: Deltadelta(ICF2CF2CF2)2=0.08, Deltadelta(ICF2CF2CF2)2=0.01, Deltadelta(ICF2CF2CF2)2=0.00. An XRD test was performed on the adduct crystal which confirmed the exclusive presence of decamethonium iodide and dodecafluoro-1,6-diiodohexane. In fact, FIG. 3 represents the crystalline structure of the adduct in which the molecules of dodecamethonium iodide (the carbon and nitrogen atoms are light grey coloured and the hydrogen atoms white) alternate with the molecules of dodecafluoro-1,6-diiodohexane (carbon atoms are light grey coloured, hydrogen atoms white and the iodine atoms dark grey) and with the iodide atoms (dark grey coloured). Moreover, it was observed that, at the crystalline state, decamethonium iodide and dodecafluoro-1,6-diiodohexane form alternating parallel layers, since the dodecafluoro-1,6-diiodohexane occupies the cavity defined by the spacer chain between the two nitrogen atoms of the dodecamethonium iodide and the two iodides of the same, due to the iodide-iodine interactions generated.Thus, the following crystallographic measurements are reported: As can be observed, in the adduct crystal, the difference Delta (B-A) between the distance B between the iodide atoms aligned with the molecule of dodecafluoro-1,6-diiodohexane, as shown in FIG. 1, and the distance A between the nitrogen atoms belonging to the same dodecamethonium molecule is equal to 0.688 A and significant of the existence of said interactions I . . . I-.The following tests were performed on the pure dodecafluoro-1,6-diiodohexane:IR (cm-1, selective bands): pure dodecafluoro-1,6-diiodohexane: 1190, 1130, 1039, 887, 763; 19F NMR (470.6 MHz, CD3OD, 0.002 M): pure do decafluoro-1,6-diiodohexane: delta=-63.80 (ICF2CF2)2, -112.02 (ICF2CF2)2. The gas chromatography tests also confirmed that this was only 100% dodecafluoro-1,6-diiodohexane.

The synthetic route of 375-80-4 has been constantly updated, and we look forward to future research findings.

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 54413-93-3, name is 2-Iodo-5-methoxybenzoic acid, A new synthetic method of this compound is introduced below., Formula: C8H7IO3

General procedure: To a solution of 2-bromo-6-methoxybenzoic acid (104 mg, 397 mumol) in CH2Cl2 (3.0 mL) were added chloromethlenedimethyliminium chloride (50.8 mg, 397 mumol) at 0 °C under Ar atmosphere, then the mixture was stirred at room temperature for 1 h. At 0 °C, 2-(4-butylaminophenyl)-1,1,1,3,3,3-hexafluoropropan-2-ol (29g)24 (50.0 mg, 159 mumol) and Et3N (166 mul, 1.19 mmol) then the mixture was stirred for 3 h, and was allowed to warm to room temperature. At 0 °C, the mixture was diluted with ethyl acetate and then water was added. The organic layer was separated and washed with brine, and dried over Na2SO4, and concentrated under reduced pressure. The residue was purified by column chromatography (n-hexane/AcOEt = 1:0-1:1) to give 30g (73.5 mg, 139 mumol, 88percent) as a colorless oil.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

6828-35-9, name is 5-Chloro-2-iodoaniline, belongs to iodides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Formula: C6H5ClIN

General procedure: 2-aminobenzenethiol (10 g, 80mmol), 3, 4-difluorobenzonitrile (11.12, 80mmol) and ferric citrate (19.59g, 80mmol) were added in DMF (50.00 mL) at 25-30 0C. The reaction mixture was heated to 110C. Reaction mixture was monitored for the synthesis of compound 3 by TLC. (2ml of reaction mixture was withdrawn and separated in ethylacetate and water. Ethyl acetate solution concentrated and crystallised in isopropyl ether to give compound 3 for characterization). After completion of reaction by TLC, powdered potassium carbonate (16.58 g, 120mmol) was added to the solution and stirred for 1 hr. The mixture was heated to 110C till completion by TLC. After completion of reaction, the mass was cooled to 25-30 C. Ethyl acetate (150 mL) and DM water (150 mL) were added. Layers separated. Organic layer washed with water (150 mL), dried over sodium sulfate and concentrated. Isopropyl ether (IPE; 150 mL) was added to the slurry, filtered, washed with IPE. Dried under vacuum at 50 C (16.84g, 94%).

The synthetic route of 6828-35-9 has been constantly updated, and we look forward to future research findings.