Month: April 2021

Reference of 52570-33-9, These common heterocyclic compound, 52570-33-9, name is Methyl 3-iodo-2-methylbenzoate, 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.

To a solution of methyl 3-iodo-2-methylbenzoate (5.20 g, 18.8 mmol) in CCI4 (90 mL) at RT was added N-bromosuccinimide (NBS) (4.02 g, 22.6 mmol) then the reaction flask was purged with N2. After the mixture was stirred at 85 C for 5 m, 2,2?-azobis(2- methylpropionitrile) (AIBN) (1.62 g, 9.42 mmol) was added. The mixture was stirred overnight at 85 C then concentrated. The residue was diluted with H2O and extracted with EtOAc. The organic phase was dried over Na2S04, filtered, and concentrated to give the crude product, which was purified using silica gel eluting with EtOAc in petroleum ether from 0% to 1% to afford methyl 2-(bromomethyl)-3-iodobenzoate (2.64 g, 40% yield) as a solid.

Statistics shows that Methyl 3-iodo-2-methylbenzoate is playing an increasingly important role. we look forward to future research findings about 52570-33-9.

Reference of 19094-56-5, 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. 19094-56-5, name is 2-Chloro-5-iodobenzoic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

The polyphosphoric acid (113 mL) was added to the three-necked flask, and the compound of formula 1b (28.25 g, 100 mmol) was added and heated to an inner temperature of about 50 C and stirred,Phenol (18.82 g, 200 mmol) was added,After heating, the temperature was raised to 80 to 85 C for 3 to 4 hours. After the reaction was cooled to 50 C, the reaction was slowly added dropwise (283 m), followed by addition of dichloromethane (169 mL)After the separation of the organic phase, the aqueous phase was extracted twice with methylene chloride (84 mL) and the combined organic phase saturated sodium bicarbonate (169 mL)The solution was washed once, washed twice with saturated brine (84 mL), dried over sodium sulfate, concentrated with a mixed solvent of dichloromethane ethanol Crystallization gave compound 2b (29.76 g, 83%).

The synthetic route of 2-Chloro-5-iodobenzoic acid has been constantly updated, and we look forward to future research findings.

Synthetic Route of 6828-35-9, 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 6828-35-9 as follows.

General procedure: A mixture of 2-iodoaniline 1 (0.5 mmol) and Pd(OAc)2 (5.6 mg, 0.025 mmol, 5.0 mol%) in CH3CN (3 mL) was added into a Schlenk flask (25 mL) and stirred at room temperature. Followed by the addition of ethyl acrylate 2a (100 mg, 1.0 mmol, 2.0 equiv) and triethylamine (101 mg, 1.0 mmol, 2.0 equiv), the mixture was stirred at 100 C until the reaction was finished. Then the mixture was filtered and the filtrate was concentrated under reduced pressure. The residue was purified by column chromatography on silica gel (petroleum ether/ethyl acetate, 5:1 to 2:1) afforded the corresponding alkenylanilines 3.

According to the analysis of related databases, 6828-35-9, the application of this compound in the production field has become more and more popular.

101335-11-9, name is 2-Chloro-4-fluoro-1-iodobenzene, 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: C6H3ClFI

7,7-Dimethyl-2-(pyridin-2-yl)-4,5,6,7-tetrahydrooxazolo[4,5-c]pyridine (460 mg, 2.0 m mol), Pd2(dba)3 (92 mg, 0.1 mmol), X-phos (95 mg, 0.2 mmol), 2-chloro-4- fluoro-1-iodobenzene (768 mg, 3.0 mmol), and Na-OtBu (576 mg, 6.0 mmol) were combined in toluene (15 mL) and heated at 1500C by microwave for 3 h. The reaction was evaporated to dryness, diluted with dichloromethane and extracted with water. The combined organic layer was dried using sodium sulfate, filtered, evaporated, and then purified by prep-TLC to obtain the title compound as a yellow solid. (6 mg, 0.87 %). 1H NMR (400 MHz, CDCl3): delta 8.74-8.76 (m, IH), 8.08-8.11 (m, IH), 7.78-7.72 (m, IH), 7.32-7.36 (m, IH), 7.15-7.20 (m, 2H), 6.96-7.01 (m, IH), 4.06 (s, 2H), 3.12 (s, 2H), 1.46(s, 6H); LC/MS: m/e = 358 (M+H)+.

The synthetic route of 101335-11-9 has been constantly updated, and we look forward to future research findings.

Electric Literature of 25309-64-2, These common heterocyclic compound, 25309-64-2, name is 1-Ethyl-4-iodobenzene, 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 large microwave tube (Biotage, 10-20 mL) equipped with a stir bar was added Pd(OAc)2(23.4 mg, 0.10 mmol, 10 mol %), S-1 (400 mg, 1.04 mmol, 1 equiv), cesium pivalate (731 mg,3.12 mmol, 3 equiv), aryl iodide (2-3 equiv) and anhydrous tert-amyl alcohol (9.6 mL). The capwas crimped and the vessel was flushed with nitrogen. The microwave tube was heated withfollowing parameters: 1 min pre-stirring, followed by a ramp (normal) to 180 C and held attemperature for 30 to 50 min. Hydrazine (500 muL of 35% aqueous) was added to the reaction andallowed to stir at 60 C for 1 hr or at room temperature overnight. The tert-amyl alcohol wasremoved en vacuo and the remaining residue dissolved with EtOAc, filtered through a plug ofcelite, and concentrated en vacuo. The crude reaction was purified via flash columnchromatography with EtOAc/Heptanes.

Statistics shows that 1-Ethyl-4-iodobenzene is playing an increasingly important role. we look forward to future research findings about 25309-64-2.

Related Products of 3032-81-3,Some common heterocyclic compound, 3032-81-3, name is 1,3-Dichloro-5-iodobenzene, molecular formula is C6H3Cl2I, 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.

2,6-diamino-9H-purine-8- thiol (3.6 mmol), neocuproine hydrate (0.36 mmol), Cul (0.36 mmol), NaO-?-Bu (7.2 mmol), 1,3- dichloro-5-iodobenzene (10.8 mmol), and anhydrous DMF (24 mL) were taken in a round bottom flask flushed with nitrogen. The flask was sealed with Teflon tape, heated at 1 10 °C, and magnetically stirred for 20 h under nitrogen. Solvent was removed under reduced pressure and the resulting residue was chromatographed (CH2Cl2:MeOH:AcOH, 20: 1 :0.5). Obtained as a light yellow solid in 65 percent yield. MS (ESI): m/z 326.9 [M + H]+.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1,3-Dichloro-5-iodobenzene, its application will become more common.

Electric Literature of 31599-61-8, 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. 31599-61-8, name is 4-Iodo-1,2-dimethylbenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: Pd cNPs/CFe3O4(20 mg, 0.73 mol%), aryl halide (0.5 mmol),phenylboronic acid (0.6 mmol), K2CO3(1.5 mmol), and EtOH (3 mL)were taken in a schlenk tube with a teflon stopcock, sealed andheated at 70C for a given time with constant stirring. For chloroderivatives, the reaction was performed using TBAB as additive(0.5 mmol), DMF (3 mL), at 110C and catalyst 40 mg (1.5 mol%).After the completion of reaction, the catalyst was separated by anexternal magnet and reaction mixture was washed with water toremove excess of boronic acids and further the mixture was sepa-rated by ethyl acetate. The solvent was evaporated and the residuewasresiduewas subjected to GC analysis (retention time of halobenzene wasused as the internal standard) followed by column chromatographyfor further purification. The purified compounds were character-ized by1H and13C NMR spectroscopy using CDCl3as solvent andTMS as internal standard. The spectral details and spectra are givenin supporting information section (Figs. S5-S24).

The synthetic route of 4-Iodo-1,2-dimethylbenzene has been constantly updated, and we look forward to future research findings.

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

Compound B (5356 kg) was suspended in a mixture of acetic anhydride and acetic acid (7760 L, 1.45 L/kg Compound B, 87 v/v % acetic anhydride and 13 v/v % acetic acid) at ambient temperature. This mixture was prepared by mixing acetic anhydride (6086 kg) and regenerated acetic anhydride (2295 kg), the latter containing 48 v/v % acetic anhydride and 52 v/v % acetic acid obtained from a previous batch. The mixture was heated to 55C. Then, p-toluene sulfonic acid (25 kg) was added and the reaction mixture was further heated to 124C over about 90 minutes. All solids were dissolved in the reaction, and 100 % of Compound B was acetylated. The remaining acetic anhydride/acetic acid (5580 L) was distilled off under reduced pressure resulting in a very viscous reaction mixture. Thirty-nine percent of the distillate could be re-used as reagent in a later batch without a discrete purification step.

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: 289039-83-4, name is Methyl 2-amino-5-bromo-3-iodobenzoate, 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 289039-83-4, COA of Formula: C8H7BrINO2

[0323] Pent-4-yn-l-ol (35.4 mg, 0.42 mmol), methyl 2-amino-5-bromo-3-iodobenzoate (100 mg, 0.28 mmol) ,PdCl2(PPh3)2 (45.9 mg, 0.06 mmol), DIEA (0.098 mL, 0.56 mmol)and copper(I) iodide (10.70 mg, 0.06 mmol) were suspended in THF (2 mL) under nitrogen. The reaction was stirred at rt for 2 hours. The solvent was removed. The crude product was purified by flash silica chromatography, elution gradient 0 to 80% EtOAc in petroleum ether. Pure fractions were evaporated to dryness to afford methyl 2-amino-5-bromo-3-(5-hydroxypent-l-yn-l-yl)benzoate (0954) (80 mg, 91 %) as a brown solid (80 mg, 91%). XH NMR (300 MHz,CDCl3-d6) delta ppm 1.67 – 1.76 (2H,m), 2.50 – 2.57 (2H, m), 3.50 – 3.82 (2H, m), 3.82 (3H, s), 4.58 (1H, tr), 6.76 (2H, brs), 7.52 (1H, d), 7.79(1H, d). LC-MS (Method A): m/z (ES+), [M+H]+ = 312.2; acid, HPLC tR = 1.54 mm.

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, Methyl 2-amino-5-bromo-3-iodobenzoate, other downstream synthetic routes, hurry up and to see.

Electric Literature of 2996-30-7, These common heterocyclic compound, 2996-30-7, name is 3-Fluoro-4-iodonitrobenzene, 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.

A solution of 2-fluoro-1-iodo-4-nitrobenzene (1.96 g, 7.34 mmol), bis(pinacolato)diboron (1.86 g, 7.34 mmol), dichloro[1,1′-bis(diphenylphosphino)ferrocene]palladium (II) dichloromethane adduct (0.599 g, 0.734 mmol), and potassium acetate (2.38 g, 24.2 mmol) in DMSO (14.7 mL) in a seal-able tube was degassed with nitrogen for 15 min, sealed, and stirred at 100 C. for 2.5 h. The reaction mixture was cooled to room temperature, diluted with water and ethyl acetate, and filtered over Celite. The aqueous layer was separated and re-extracted with ethyl acetate. The combined organic layers were washed with brine, dried over magnesium sulfate, filtered, and concentrated to a brown oil. Purification by flash column chromatography using ethyl acetate in hexanes (0%-20%) gave the desired product (1.60 g, 81.6%).

The synthetic route of 2996-30-7 has been constantly updated, and we look forward to future research findings.