Category: iodides-buliding-blocks

Reference of 4949-69-3, A common heterocyclic compound, 4949-69-3, name is 4-Iodo-3-methylaniline, molecular formula is C7H8IN, its 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.

General procedure: A mixture of CuCl (5 g, 50.5 mmol) and pyridine (50 mL) was stirred at r.t. for 30 min. The suspension was filtered and the halogenated aniline (1.5 equiv) was added to the green solution. Air was bubbled through the solution for 18 h. The residue was diluted with CH2Cl2 (200 mL) and aq 1 M HCl (100 mL). The aqueous layer was extracted with CH2Cl2 (3 × 100 mL). The combined organic layers were washed with H2O (100 mL), dried (MgSO4), and concentrated.The crude product was recrystallized from EtOH.

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.

Application of 20691-72-9, 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. 20691-72-9, name is 4-Iodo-2-nitroaniline belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Method b: To a mixture of the 4-iodo-2-nitroaniline (142 mmol) and cesium carbonate (55.5 g, 170 mmol) in 2-butanone (740 mL) was dropwise added a solution of Boc2O (37.8 g, 173 mmol) in 2-butanone (170 mL) and the resulting mixture was stirred at 52 C. for 26 h. The solvent was removed in vacuum, the residue was treated with a mixture of H2O (240 mL) and MeOH (240 mL) and extracted with hexane (3*500 mL). The combined hexane layer was washed with brine (200 mL) and all aqueous layers were reextracted with hexane (300 mL). All combined hexane layers were dried over MgSO4, filtered and the solvent was removed in vacuum to give an orange solid, which was purified by silica gel column chromatography with hexane/EtOAc to give the (4-iodo-2-nitro-phenyl)-carbamic acid tert.-butyl ester as a yellow solid.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 4-Iodo-2-nitroaniline, other downstream synthetic routes, hurry up and to see.

Application of 14452-30-3, A common heterocyclic compound, 14452-30-3, name is 1-(3-Iodophenyl)ethanone, molecular formula is C8H7IO, its 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.

General procedure: Aryl halide (1 mmol), phenylacetylene (1.5 mmol), and PNIPAM-co-PPAP/Pd catalyst (0.1 mol% Pd based on Aryl halide) were added into a 10 mL overpressure screw-capped vial equipped with a magnetically stirring bar, and then 1 mL deionized water was added. After the mixture was degassed under argon gas for 10 min, Et3N (3 mmol) was added in, and the solution was stirred at a given temperature for appropriate time. After the reaction was completed and cooled to room temperature, the solution was diluted with deionized water, and extracted with ethyl acetate (3 × 6 mL). The organic phase was washed with brine, dried with MgSO4, and then the solvent was evaporated under reduced pressure. The resulting residue was chromatographed on silica gel (hexane/ethyl acetate) to give pure product which was analyzed by 1H and 13C NMR, and the specific data were shown in Supporting Information.

The synthetic route of 14452-30-3 has been constantly updated, and we look forward to future research findings.

Application of 25309-64-2, A common heterocyclic compound, 25309-64-2, name is 1-Ethyl-4-iodobenzene, molecular formula is C8H9I, its 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.

General procedure: Under nitrogen atmosphere, Cu2O (10 mol %), DABCO (25 mol %), and a stirring bar were added into a 10 mL oven-dried sealed glass tube (as shown in Figure S1). Then NMP (0.5 mL), aryl iodides (0.125 mmol, 1.0 equiv.) and PhSiH3 (0.75 mmol, 6 equiv.) were injected by syringe. The tube was then sealed and CO2 (0.67 mmol, 5.4 equiv., 15 mL) as well as NH3 (0.67 mmol, 5.4 equiv., 15 mL) were injected by syringe after N2 was removed under vacuum. Finally, the mixture was stirred for 24 hr in a pre-heated-to-130 C alloyed block. After the reaction was finished, the tube was cooled to room temperature and the pressure was carefully released. The yield of were measured by GC analysis using dodecane as the internal standard or by flash chromatography on silica gel (petroleumether/ethyl acetate).

The synthetic route of 25309-64-2 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. 52807-27-9, name is 4-Chloro-2-iodoanisole, A new synthetic method of this compound is introduced below., Product Details of 52807-27-9

EXAMPLE 37A 3′,5-dichloro(1,1′-biphenyl)-2-yl methyl ether A suspension of 4-chloro-2-iodo-1-methoxybenzene (2.5 g, 9.3 mmol) and 3-chlorophenylboronic acid (2.2 g, 13.9 mmol) in a mixture of toluene (10 mL), dioxane (10 mL), and 2N Na2CO3 (10 mL) was treated with tetrakis(triphenylphosphine)-palladium (O) (0.54 g, 0.47 mmol), heated to reflux for 16 hours, cooled to room temperature, and extracted with ethyl acetate. The combined extracts were dried (MgSO4), filtered, and concentrated. The concentrate was purified by flash column chromatography on silica gel with 20:1 hexanes/ethyl acetate to provide 2.5 g (100%) of the desired product. MS (DCI/NH3) m/z 254 (M+H)+; 1H NMR (CDCl3) delta 7.75-7.23 (m, 6H), 6.91 (d, 1H), 3.80 (s, 3H).

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: 481075-58-5, name is 2-Bromo-1-iodo-4-(trifluoromethyl)benzene, 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 481075-58-5, Recommanded Product: 481075-58-5

Under the protection of nitrogen, the 2-bromo-1-iodo-4 – (trifluoromethyl) benzene (0.50g, 1 . 42mmol), 4 – (4, 4, 5, 5-tetramethyl -1, 3, 2- two oxygen boron fifth heavenly stem link -2-yl) – 5,6-dihydropyridine -1 (2H)-carboxylic acid tert-butyl (0.48g, 1 . 57mmol), Pd (PPh3)2Cl2(25 mg, 36 mumol) and sodium carbonate (0.23g, 2 . 14mmol) into acetonitrile (10 ml) and water (3 ml) in the mixed solvent. Reaction solution is heated to 90 C stirring for 12 hours, cooling to the room temperature and adding water (20 ml), then with ethyl acetate (20 ml × 3) extraction. Combined organic phase dried with anhydrous sodium sulfate, filter, and concentrating under reduced pressure, the resulting residue by a silica gel column chromatography (petroleum ether/ethyl acetate (v/v)=20/1) to obtain the title compound as a yellow oily liquid (470 mg, 81.0%).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2-Bromo-1-iodo-4-(trifluoromethyl)benzene, and friends who are interested can also refer to it.

Reference of 461-17-6,Some common heterocyclic compound, 461-17-6, name is 1,1,1-Trifluoro-4-iodobutane, molecular formula is C4H6F3I, 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.

1.4 g of 2- (2, 2,3, 3,4, 4,5, 5- octafluoropentyl) malononitrile and 1.2 g of 1-iodo-4, 4,4- trifluorobutane were dissolved in 5 ml of dimethyl sulfoxide, 0.83 g of potassium carbonate was added, and the mixture was stirred at room temperature for 5 hours. Thereafter, dilute hydrochloric acid was added to the reaction mixture, followed by extraction with methyl tert- butyl ether. The organic layer was washed successively with water, aqueous saturated sodium hydrogen carbonate and aqueous saturated sodium chloride, dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to obtain 0.35 g of 2- (2, 2,3, 3,4, 4,5, 5- octafluoropentyl)-2- (4, 4,4-trifluorobutyl) malononitrile (hereinafter, referred to as the present compound (66)). The present compound (66): lH-NMR (CDCl3, TMS) b (ppm): 2.01-2. 13 (2H, m), 2. 16-2. 32 (4H, m), 2.78 (2H, t), 6.02 (1H, tt).

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

In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 71838-16-9 as follows. Recommanded Product: 2-Bromo-1-iodo-4-methylbenzene

Step A. 4-(2′-bromo-4′-methylbiphenyl-4-yl)-1-(2,2,2-trifluoroethyl)piperidine A mixture of 2-bromo-1-iodo-4-methylbenzene (0.764 g, 2.57 mmol), the title compound from Example 60 Step B (1.00 g, 2.71 mmol), dichloro bis(triphenylphosphine)palladium(II) (0.095 g, 0.135 mmol), sodium carbonate (5.42 mL of 1 M solution, 5.42 mmol) and MeCN (5.42 mL) was heated at 110 C. overnight. Organic layer was separated. Aqueous layer was extracted with hexanes-EtOAc. The organic layers were combined and concentrated. Silica gel flash chromatography eluting with hexanes:EtOAc (20:1 to 9:1 v/v) gave the title compound: LCMS m/z 414.0 [M+H+]; 1H NMR (500 MHz, CDCl3) delta 7.54 (s, 1H), 7.40 (d, J=8.1 Hz, 2H), 7.31 (d, J=8.1 Hz, 2H), 7.26 (d, J=7.8 Hz, 1H), 7.20 (d, J=7.8 Hz, 1H), 3.16 (m, 2H), 3.08 (q, J=9.8 Hz, 2H), 2.57 (m, 3H), 2.42 (s, 3H). 1.95-1.88 (m, 4H).

According to the analysis of related databases, 71838-16-9, the application of this compound in the production field has become more and more popular.

69113-59-3, name is 3-Iodobenzonitrile, 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. Application In Synthesis of 3-Iodobenzonitrile

Example 173-Trimethylsilanylethynyl-benzonitrile 3-Iodo-benzonitrile (10.0 g, 43.7 mmol), trilmethylsilane acetylene (5.57 g, 56.8 mmol), palladium tetrakis triphenylphosphine (2.02 g, 1.75 mmol), and copper iodide (1.0 g, 5.24 mmol) in triethylamine (120 mL) was stirred for 12 h. The reaction was concentrated and purified by column chromatography to afford the title product (9.35 g, quantitative yield) as a brown oil.1H NMR (300 MHz, CDCl3): delta (ppm) 7.76 (t, 1H), 7.71 (dd, 1H), 7.63 (dd, 1H), 7.28 (t, 1H), 0.26 (s, 9H).

The synthetic route of 69113-59-3 has been constantly updated, and we look forward to future research findings.

Adding a certain compound to certain chemical reactions, such as: 4387-36-4, name is 2-Iodobenzonitrile, 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 4387-36-4, name: 2-Iodobenzonitrile

This compound was prepared by following aliterature procedure.2 A solution of o-iodobenzonitrile(0.916 g, 4 mmol) in THF (0.5 mL)was added drop-wise to 1 M LiN(SiMe3)2 in anhydrous THF (4.4 mL, 4.4mmol) at room temperature and the reaction mixture was stirred at sametemperature overnight. i-PrOH (3 mL) was added and thecrude reaction mixture was bubbled with HCl (gas) for 15 min. The mixture waskept at 0 °C overnight. The precipitated product was filtered and washed withdiethyl ether to yield titled product as a white solid (0.961 g, 85percent). Mp291°C; 1H NMR (500 MHz, DMSO-d6) delta 8.90 (s, 4H), 8.01 (dd, J = 8.0, 1.0 Hz, 1H), 7.63 ? 7.49 (m,2H), 7.35 (ddd, J = 7.9, 7.2, 2.0 Hz,1H); 13C NMR (126 MHz, DMSO) delta 167.64, 139.23, 135.90, 132.71,128.92, 128.27, 94.88; IR (neat) 3038, 1664, 1588, 1404 cm-1; HRMScalcd for C7H8IN2 (M++1) + [-HCl]:246.9727, found 246.9719.

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.