Month: April 2021

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.

Reference of 181765-86-6, A common heterocyclic compound, 181765-86-6, name is Methyl 5-bromo-2-iodobenzoate, molecular formula is C8H6BrIO2, 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.

Example 5 [00619] Preparation of Cpd 30 [00620] Step A: A mixture of methyl 5-bromo-2-iodobenzoate (18.4 g, 54.0 mmol), TMS acetylene (8.5 mL, 5.88 g, 60.0 mmol), Cul (0.51 g, 2.7 mmol), PdCl2(Ph3P)2 (1.9 g, 2.7 mmol), Et3N (15.0 mL, 10.9 g, 108.0 mmol) and acetonitrile (100 mL) was stirred under argon at room temperature for 4 hours. After the removal of the volatiles in vacuo, the residue was chromatographed (silica gel, ethyl acetate in hexanes, 0-20%) to provide the TMS alkyne intermediate as colorless oil (15.7 g, 94%).

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 610-97-9, A common heterocyclic compound, 610-97-9, name is Methyl 2-iodobenzoate, molecular formula is C8H7IO2, 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 50mL round-bottomed flask equipped with a gas inlet tube, a reflux condenser, and a magnetic stirring bar was charged with MCM-41-S-PdCl2 (173mg, 0.05 mmol Pd), aryl halide (5.0 mmol) and HCOONa (7.5 mmol). The flask was flushed with carbon monoxide. DMF (5 mL) was added by syringe and a slow stream of CO was passed into the suspension. The mixture was vigorously stirred at 100-110C for 4-24h, cooled to room temperature, and diluted with diethyl ether (50 mL). The palladium catalyst was separated from the mixture by filtration, washed with distilled water (2×10 mL), ethanol (2×10 mL) and ether (2×10 mL) and reused in the next run. The ethereal solution was washed with water (3×20mL) and dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was purified by flash column chromatography on silica gel (hexane-ethyl acetate=10:1). (0008) All formylation products were characterized by comparison of their spectra and physical data with authentic samples. IR spectra were determined on a Perkin-Elmer 683 instrument. 1H NMR (400MHz) and 13C NMR (100MHz) spectra were recorded on a Bruker Avance 400MHz spectrometer with TMS as an internal standard and CDCl3 as solvent.

The synthetic route of 610-97-9 has been constantly updated, and we look forward to future research findings.

Adding a certain compound to certain chemical reactions, such as: 7425-53-8, name is Ethyl 4-iodobutanoate, 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 7425-53-8, SDS of cas: 7425-53-8

Ethyl ester 4-Et. DIEA (11.8 g, 91.7 rnmol) was added to a mixture of compound 3 (13.9 g, 45.87 mmol) and ethyl 3- iodobutyrate (13.3 g, 55.05 minol) in a screw-cup bottle, and the reaction mixture was stirred with heating (110 C) for 2 days. After cooling, the reaction mixture was diluted with diethyl ether, passed through a plug of silica gel (eluting with ether), and the filtrate evaporated in vacuo. The residue was dissolved in hexane/ether (3/1) mixture, washed with water, brine and dried over MgSO4. The product 4-Et was isolated by a short path column chromatography (hexane-hexane/ether 10/1; Rf = 0.59 in hexane/ether = 10/1); yield 18.75 g (98.5%) of a clear oil. ?H NMR (300 MHz, CDC13): delta = 0.21 (s, 6 H, SiMe2But), 0.98 (5, 9 H, SiMe2But), 1.26 Ct, J = 7.2 Hz, 3 H, CO2CH2CH3), 1.28 Cs, 6 H, 2xMe), 1.90 Cm, 2 H, NCH2CH2CH2CO2Et), 1.93 (d, J = 0.5 Hz, 3 H, Me), 2.38 Cm, 2 H, NCH2CH2CH2CO2Et), 3.20 (m, 2 H, NCF{2CH2CH2CO2Et), 4.16 (q, J = 7.2 Hz, 2 H, CO2CH2CH3), 5.10 (d, J = 0.5 Hz, 1 H, HC=), 6.02 Cm, 1 H), 6.10 Cm, 1 H), 6.90 Cm, 1 H) ppm.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Ethyl 4-iodobutanoate, and friends who are interested can also refer to it.