Iodides-buliding-blocks

Electric Literature of 1450754-38-7, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 1450754-38-7 name is 3-(But-3-yn-1-yl)-3-(2-iodoethyl)-3H-diazirine, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

K2CO3 (0.207g, 1.5 mmoL) and L3 (0.248g, 1.0 mmoL) were added orderly to a solution of phenol (0.113g, 1.2 mmoL) in DMF (10mL). The reaction mixture was stirred at 50C for 16h and monitored by TLC. The reaction was quenched by adding H2O (5mL). The crude product was exacted into EtOAc (3×10mL). The combined organic layers were washed with brine (10mL), and dried over Na2SO4 and then filtered. The filtrate was concentrated under reduced pressure. The residue was purified by flash column chromatography giving NP as colorless oil (171mg, yield 80%). 1H NMR (300MHz, CDCl3) delta 7.34-7.28 (m, 2H), 7.01-6.95 (m, 1H), 6.94-6.88 (m, 2H), 3.85 (t, J=6.2Hz, 2H), 2.13-2.06 (m, 2H), 2.01 (t, J=2.6Hz, 1H), 1.91 (t, J=6.2Hz, 2H), 1.80-1.73 (m, 2H). 13C NMR (75MHz, CDCl3) delta 158.4, 129.5, 121.1, 114.5, 82.8, 69.2, 62.4, 33.0, 32.7, 26.7, 13.3. Purity: 97.13% by (0.01M KH2PO4 solution: MeOH=15: 85).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3-(But-3-yn-1-yl)-3-(2-iodoethyl)-3H-diazirine, and friends who are interested can also refer to it.

These common heterocyclic compound, 887266-99-1, name is 3-Fluoro-4-iodobenzonitrile, 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. HPLC of Formula: C7H3FIN

A mixture of 3-fluoro-4-iodobenzonitrile (1.0 g, 4.06 mmol), trimethylsilyl acetylene (0.595 g,6.07 mmol), CuT (50 mg, 0.26 mmol), PdC12(PPh3)2 (50 mg, 0.07 1 mmol) and TEA (3 mL) in DMSO (7 mL) was stirred at RT for 16 h. After the reaction, the reaction mixture was quenched with water, extracted with EtOAc. The organic layer was washed with water, brine, dried over Na2SO4 and concentrated to afford 750 mg of crude 2-chloro-5-((trimethylsilyl)-ethynyl) benzoate. To this crude solution of 2-chloro-5-((trimethylsilyl)ethynyl)benzoate (500 mg, 1.87 mmol) in DCM (10 mL) was added TBAF (1.0 g, 3.83 mmol) and stirred further at RT for h. Then the reaction mixture was quenched with water, extracted with DCM, washed with water, brine, dried over Na2SO4 and concentrated to afford 450 mg of the title product. ?H NMR (300 MHz, CDC13): 7.61-7.56 (t, J= 7.2 Hz, 1H), 7.44-7.38 (d, J= 8.1 Hz,2H), 3.52(s, 1H).

The synthetic route of 3-Fluoro-4-iodobenzonitrile has been constantly updated, and we look forward to future research findings.

Reference of 39998-81-7, 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 39998-81-7 as follows.

2-Fluoro-4-iodobenzoic acid (Compound B) A round bottom (RB) flask containing a solution of 8.0 g (27.0 mmol) of sodium dichromate in 44 mL of glacial acetic acid was placed in an external water bath (21 C.) and left exposed to air. To the resultant orange slurry was added 3.2 g (13.6 mmol) of 2-fluoro-4-iodotoluene followed by the dropwise addition of 22 mL of c. sulfuric acid via syringe (caution: if added too quickly there is a tendency for the mixture to erupt). After the addition of approximately 8 mL of sulfuric acid, a green solid precipitated and the water bath temperature had risen (25 C.). The green reaction mixture was heated in an oil bath (90 C.) for one hour, allowed to cool to ambient temperature, diluted with 1N NaOH solution (aq.) and ethyl acetate (500 mL) and then quenched with sat. NaHCO3 (aq.) solution. The organic phase was separated and washed with water and brine, dried over MgSO4, filtered and concentrated in vacuo to an orange oil. Residual acetic acid was removed by further extraction between ethyl acetate and sat. NaHCO3 (aq.) solution and washing of the organic phase with water and brine. The organic phase was dried over MgSO4, filtered and concentrated in vacuo to give the title compound as an orange solid. PMR (DMSO-d6): delta 7.61 (1H, t, J=8.0 Hz, J (C–F)=8.0 Hz), 7.67 (1H, dd, J=1.5, 8.2 Hz), 7.78 (1H, dd, J=1.5 Hz, J (C–F)=8.9 Hz).

According to the analysis of related databases, 39998-81-7, the application of this compound in the production field has become more and more popular.

39998-81-7, name is 2-Fluoro-4-iodo-1-methylbenzene, 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. COA of Formula: C7H6FI

To a solution of 2-fluoro-4-iodotoluene (2.83 g, 12 mmol) in Cd4 (120 mL) were added NBS (2.24 g, 12.6 mmol) and BPO (0.06 g, 0.24 mmol). The reaction mixture was refluxed for 9 h under N2, then cooled to rt and concentrated in vacuo. The residue was purified by a silica gel column chromatography (PE) to give the title compound as a white solid (2.16 g, 57%).

The synthetic route of 39998-81-7 has been constantly updated, and we look forward to future research findings.

Related Products of 76801-93-9,Some common heterocyclic compound, 76801-93-9, name is 5-Amino-N1,N3-bis(2,3-dihydroxypropyl)-2,4,6-triiodoisophthalamide, molecular formula is C14H18I3N3O6, 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.

Compound B was acetylated in a mixture of acetic anhydride and acetic acid in the presence of catalytic amounts of p-toluene sulphonic acid at 50-125 C. Excess acetic anhydride and acetic acid was distilled off under reduced pressure, and the reaction mixture was diluted with methanol and water. The resulting reaction mixture had the following composition:Overacetylated Compound A (a mixture of compounds with varying number of acetyl groups attached): 97.7-98.3% by area in HPLCCompound B: 0.0-0.3% by area in HPLCConcentration: 31 w/v % Compound A in an approximately 2.5:1 methanol/water mixtureConductivity: 5.1-5.7 mS/cmCompound B was produced from the reaction mixture in a system according to FIG. 1. The reaction mixture from the acetylation reaction (prepared batch wise) was fed into the static mixer in a flow ratio of 1.04 mL reaction mixture:1.0 mL 20 w/w % NaOH at about 55 C. (outlet temperature). The absolute feeding rate of the reaction mixture was 2.6 kg/hour. The pH was kept at about 12.2 at steady state. HPLC of the output stream showed Compound A in 98.2% purity with 0.23% Compound B present at steady state.The continuous crystallisation was performed as described above. The pH in the first and second crystalliser varied between 11.1 and 11.5 over time, while the pH in the third and fourth crystalliser varied between 6.2 and 7.2. The temperature was 60 C. in the two first crystallisers and 20 C. in the third and fourth. Residence times were held at 2, 2, 2 and 8 hours, respectively. 20% of the mother liquor volume was stripped off in the third crystalliser at a pressure of 240-250 mbar. The water content in the methanolic distillate from the stripping was 34-35 w/w %. The resulting slurry from the fourth crystalliser was transferred to a holding tank before filtration.The slurry was filtered in a continuous rotation filter at 1.6-3.2 barA. The filtration rate varied between about 500 and 900 L/m2/hour (about 500-650 L/m2/hour at steady state). The filter cake was washed with methanol (about 1.9 kg/kg Compound A) in the same filter. The resulting salt content in the filter cake was 0.2-0.3 w/w % NaCl.The moist filter cake was dried in a continuous fluid bed (spin flash) dryer at 120-130 C. gas temperature. The maximum temperature exposed to the product was 80 C. The resulting moisture content was 0.4 w/w %.The purity of dry Compound A in HPLC was 99.5% by area.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 5-Amino-N1,N3-bis(2,3-dihydroxypropyl)-2,4,6-triiodoisophthalamide, its application will become more common.

Related Products of 103962-05-6, 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. 103962-05-6, name is 1-Iodo-4-(trifluoromethoxy)benzene, This compound has unique chemical properties. The synthetic route is as follows.

General procedure: Under an argon atmosphere, nickel oxide (0.1 mmol, 10 molpercent), triphenylphosphine (0.2 mmol, 20 molpercent), iminodibenzyl substrate (1 mmol), potassium tert-butoxide (2 mmol, 2.0 equiv) were sequentially 4-trifluoromethoxyhalogenated aromatic hydrocarbon (2 mmol, 2.0 equiv) and tetrahydrofuran (2 mL) were added to a 10 mL sealed tube and placed in a 100° C. oil bath with heating and stirring for 24 hours. The reaction was completed and the reaction was exposed to air quenching. , and then directly separated by column chromatography to obtain amine products.According to the results of column chromatographic separation, the yields of 4-trifluoromethoxybromobenzene and 4-trifluoromethoxy iodobenzene respectively reacted with the substrate were 78percent and 69percent, respectively;

The chemical industry reduces the impact on the environment during synthesis 1-Iodo-4-(trifluoromethoxy)benzene. I believe this compound will play a more active role in future production and life.

Related Products of 21740-00-1,Some common heterocyclic compound, 21740-00-1, name is 5-Bromo-2-iodobenzoic acid, molecular formula is C7H4BrIO2, 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.

A mixture of 5-bromo-2-iodobenzoic acid (2) (800 mg, 2.447 mmol) and 3.5 mL of thionyl chloride was refluxed with stirring for 1 h under a N2 atmosphere, then excess of thionyl chloride was removed in vacuo. Under N2 atmosphere, sodium azide (191 mg, 2.9 mmol) and dry acetone (7 mL) were poured into the flask containing the crude acyl chloride and the mixture was stirred at room temperature for 10 min, after that, acetone was removed in vacuo. CAUTION, the acyl azide is potentially explosive, the solution should not be evaporated to complete dryness. The residue was dissolved in dry toluene (7 mL) and the mixture was stirred at 80-85 C for 3.5 h under a N2 atmosphere. To the reaction flask was added benzyl alcohol (258.0 muL, 2.5 mmol) and 4-dimethylaminopyridine (DMAP, 7.5 mg, 0.06 mmol), the resulting mixture was again stirred at 80-85 C for 1 h under N2 atmosphere. The reaction mixture was diluted with ethyl acetate and after the usual aqueous work up, the organic layer was concentrated to yield a solid residue. This solid was dissolved in dichloromethane and then petroleum ether was added to precipitate the product which was triturated and washed with dichloromethane/petroleum ether mixture to afford (3) 861 mg, 81% yield.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 5-Bromo-2-iodobenzoic acid, its application will become more common.

Reference of 3930-83-4, These common heterocyclic compound, 3930-83-4, name is 2-Iodobenzamide, 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: To a 25ml Schlenk tube containing a solution of 1 in 2ml of THF was added amide (1.0 mmol) and (EtO)3SiH (0.50 g, 3.0 mmol). The reaction mixture was stirred at 60 C until there was no amide left (monitored by TLC and GC-MS). The product was purified according to literature procedures by Beller [27].

The synthetic route of 3930-83-4 has been constantly updated, and we look forward to future research findings.

Application of 52570-33-9, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 52570-33-9 name is Methyl 3-iodo-2-methylbenzoate, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

Process using Pd Catalyst Under a nitrogen atmosphere, palladium acetate (223 mg, 0.99 mmol) , 4, 5-bis (diphenylphosphino) -9, 9-dimethylxanthene (Xantphos) (575 mg, 0.99 mmol) and toluene (62 ml) were mixed, and the mixture was stirred at room temperature for 15 minutes. To this solution, 2-amino-3-bromo-5-methylpyridine (6.20 g, 33.15 mmol), methyl 3-iodo-2-methylbenzoate (9.15 g, 33.15 mmol) and cesium carbonate (15.12 g, 46.41 mmol) were added. The mixture was stirred at an internal temperature of 100 to 105C for 7 hours. The reaction solution was cooled to room temperature, and water (50 ml) and toluene (50 ml) were added thereto. The organic layer was separated and washed sequentially with water (40 ml) and 10% brine (40 ml) . Silica gel (6 g) was added to the organic layer, the mixture was filtered, and the filtrate was concentrated under reduced pressure. Ethyl acetate (0.5 ml) and n-hexane (6 ml) were added to the concentrate, and the mixture was stirred at room temperature for 30 minutes. The crystals were collected by filtration, washed with ethyl acetate/n-hexane (1/12, 5 ml), and dried under reduced pressure at 40C, to yield the title compound (4.81 g) (yield 43.3%). 1H-NMR (CDCl3, TMS, 300 MHz) delta (ppm) : 2.23 (3H, s) , 2.52 (3H, s), 3.91 (3H, s), 6.78 (IH, brs) , 7.27 (IH, t, J = 8.0 Hz), 7.57-7.62 (2H, m) , 7.95 (IH, d, J = 1.1 Hz), 8.10 (IH, dd, J = 1.0 Hz, 8.1 Hz) .High resolution mass spectrometry Theoretical value: 334.0317 [M+] Measured value: 334.0313 [M+]Melting point: 63.9 to 64.7C

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Methyl 3-iodo-2-methylbenzoate, and friends who are interested can also refer to it.

Adding a certain compound to certain chemical reactions, such as: 199786-58-8, name is (5-Bromo-2-iodophenyl)methanol, 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 199786-58-8, Computed Properties of C7H6BrIO

To a stirred solution of PDC (11.0 g, 0.0288 mol) in CH2Cl2 (60 mL) was added a solution of 11 (4.50 g, 0.0144 mol) in CH2Cl2 (20 mL). The mixed content was stirred for 4 h at rt. The solvent was then removed under vacuum to give the crude product of 12, which was purified by silica flash column chromatography (hexanes/CH2Cl2, 7:3) to give compound 12 (4.40 g, 0.0142 mol, 98%) as a white solid.

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.