Month: May 2021

Application of 624-75-9, 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. 624-75-9 name is 2-Iodoacetonitrile, 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.

First, a stirrer was placed in a 35 mL sealed tube, and 35 muL of styrene (0.3 mmol), 1.0 ml of acetonitrile, and 44 muL of iodoacetonitrile (0.60 mmol) were added thereto, and 5·4 mg of Phen was added to the mixed solution. (0·03mmol), 5.7mgCul (0.03mmol) and 91yL DBU (0.60mmol), tightly seal the nozzle with a cock, heat to 110 C, stir for 1.5 hours, after the reaction is finished, the system is cooled to room temperature, into the reaction system 2 ml of distilled water was added, and the mixture was extracted with ethyl acetate. The organic phases were combined, and the solvent of the organic phase was evaporated under reduced pressure.36.5 mg of a colorless liquid product 3a was obtained by silica gel column chromatography, yield 85%.

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

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 628-77-3 as follows. Formula: C5H10I2

A solution of tert-butyl (11S,11aS)-8-hydroxy-7-methoxy-2-methylene-5-oxo-11-((tetrahydro-2H-pyran-2-yl)oxy)-2,3,11,11a-tetrahydro-1H-benzo[e]pyrrolo[1,2-a][1,4]diazepine-10(5H)-carboxylate 46 (200 mg, 0.43 mmol) in DMF (5.0 mL) was added K2CO3 (60 mg, 0.43 mmol) and 1,5-diiodopentane (703 mg, 2.17 mmol). The reaction mixture was stirred at 90 C. for 12 h. The reaction mixture was concentrated and purified by silica chromatography (0-50% EtOAc in petroleum ether) to give tert-butyl (11S,11aS)-8-((5-iodopentyl)oxy)-7-methoxy-2-methylene-5-oxo-11-((tetrahydro-2H-pyran-2-yl)oxy)-2,3,11,11a-tetrahydro-1H-benzo[e]pyrrolo[1,2-a][1,4]diazepine-10(5H)-carboxylate 47 (129 mg, 0.191 mmol, 43.9% yield) as a yellow oil. LCMS (5-95AB/1.5 min): RT=0.907 min, [M+H]+ 657.1

According to the analysis of related databases, 628-77-3, the application of this compound in the production field has become more and more popular.

Related Products of 755027-18-0, 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. 755027-18-0 name is 1-Bromo-4-iodo-2-methoxybenzene, 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.

General procedure: To a degassed solution of 1-bromo-4-iodo-2-methoxybenzene (2.2 g, 7.03 mmol), (4-methoxy-2-nitrophenyl)boronic acid (2.1 g, 10.55 mmol) in DME (80 mL) was added Pd(Ph3P)4 (812 mg, 0.7 mmol) and CsF (2.4 g, 15.82 mmol) under nitrogen. The reaction was then heated to 70 C for 18 h. The reaction was then extracted with EtOAc and water. The organic layer was washed with brine, dried over Na2SO4, and concentrated in vacuo. The residue was purified silica (gradient elution, 3-40% EtOAc/hexanes) to give the title compound (2.7 g, 99%).

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

Adding a certain compound to certain chemical reactions, such as: 645-00-1, name is 1-Iodo-3-nitrobenzene, 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 645-00-1, Recommanded Product: 1-Iodo-3-nitrobenzene

General procedure: An aryl halide (1.0 mmol) and a terminal alkyne (1.2 mmol) were added to a mixture of PS-dtz-Pd(II) (0.001 mmol), piperidine (2.0 mmol), and water (3 ml) in a glass flask under vigorous stirring. The mixture was stirred at room temperature for 3 h under aerobic conditions. After completion of the reaction, the mixture was filtered to recover the catalyst. The polymer was washed with water and acetonitrile, vacuum dried, and stored for a new run. After GC analysis, the solvent was removed under vacuum, and the crude product was subjected to silica gel column chromatography using CHCl3-CH3OH (97:3) as eluent to afford the pure product.

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, 1-Iodo-3-nitrobenzene, other downstream synthetic routes, hurry up and to see.

Application of 2265-91-0,Some common heterocyclic compound, 2265-91-0, name is 1,3-Difluoro-5-iodobenzene, molecular formula is C6H3F2I, 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.

Intermediate 4: Ethyl 1-(3,5-difluorophenyl)-5-methyl-1/-/-1 ,2,3-triazole-4-carboxylate; To a mixture of 1 ,3-difluoro-5-iodobenzene (0.2 g, 0.833 mmol) and ethyl 2- butynoate (0.097 ml, 0.833 mmol) in water/DMSO (0.22ml/2ml) at room temperature was added L-proline (0.019 g, 0.167 mmol), sodium carbonate (0.018 g, 0.167 mmol), sodium azide (0.065 g, 1.000 mmol), sodium l-ascorbate (0.017 g, 0.083 mmol) and copper(ll) sulfate pentahydrate (10.40 mg, 0.042 mmol) (in this order) and the mixture was heated at 65C overnight. Monitoring by LC/MS revealed starting material to be present and so the temperature was increased to 100 degrees and the mixture was heated overnight at lOOdegC. On cooling to room temperature, the mixture was quenched with aqueous ammonia (1 ml) and EtOAc (20ml) and water (20 ml) were added. The two phases were separated, and the aqueous phase was extracted with EtOAc (3x 30 ml). All organic phases were combined and washed with water/brine (50ml) repeatedly. The organic phase was dried over sodium sulfate, filtered and the solvent was evaporated to give a crude product that was purified by MDAP to afford the title compound (14.9%); MH+=267.9.

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-Difluoro-5-iodobenzene, its application will become more common.

Electric Literature of 52807-27-9, 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. 52807-27-9, name is 4-Chloro-2-iodoanisole belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Under a nitrogen atmosphere, tris (dibenzylideneacetone) dipalladium (2.29 g, 2.5 mmol) , 1, V -bis (diphenylphosphi.no) ferrocene (2.11 g, 5 mmol) , sodium tert-butoxide (6.73 g, 70 mmol) and toluene (150 ml) were mixed. To this solution, 2-amino-3-bromo-5-methylpyridine (9.82 g, 52.5 mmol), 4-chloro-2-iodo-l-methoxybenzene (13.42 g, 50 mmol) and toluene (100 ml) were added. The mixture was stirred at an internal temperature of 9O0C for 2 hours. The reaction solution was cooled to room temperature, and IN hydrochloric acid (150 ml) was added thereto. The insoluble was filtered off and washed twice with toluene (50 ml) . The organic layer was separated and washed sequentially, once with 5N aqueous sodium hydroxide solution (50 ml) and twice with water (50 ml) . The organic layer was concentrated under reduced pressure, ethanol/acetone (4/1, 30 ml) was added to the concentrate, and the crystals were collected by filtration. The crystals were washed three times with ethanol/acetone (4/1, 15 ml) , and dried under reduced pressure at 50C, to yield the title compound (12.88 g) (yield 78.6%).1H-NMR (CDCl3, TMS, 300 MHz) delta (ppm) : 2.23 (3H, s) , 3.92 (3H, s), 6.77 (IH, d, J = 8.6 Hz), 6.87 (IH, dd, J = 2.5 Hz, 8.6 Hz), 7.59 (IH, d, J = 1.5 Hz), 7.75 (IH, brs) , 8.05 (IH, d, J = 1.0 Hz), 8.69 (IH, d, J = 2.5 Hz). 13C-NMR (CDCl3, TMS, 75 MHz) delta (ppm): 17.1, 56.2, 106.8, 110.4, 117.1, 120.1, 125.4, 126.0, 131.2, 140.9, 146.0, 146.3, 149.3.Mass analysis (Ci3Hi2N2OBrCl) Theoretical value: 326 Measured value: 327 [M+H]+Elemental analysis (Ci3Hi2N2OBrCl)Theoretical value: C, 47.66; H, 3.69; N, 8.55; Br, 24.39; Cl , 10 . 82Measured value: C, 47.94; H, 3.62; N, 8.68; Br, 24.36; Cl, 10.86Melting point: 140.2C

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-Chloro-2-iodoanisole, other downstream synthetic routes, hurry up and to see.

Electric Literature of 25245-35-6, A common heterocyclic compound, 25245-35-6, name is 2-Iodo-1,4-dimethoxybenzene, molecular formula is C8H9IO2, 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 the styrene (3 mmol), the halogenated benzene (3 mmol), triethanolamine (3 mmol) and Pd(II) acetate (0.03 g) was stirred under argon at 100 C for 24 h. The reaction was cooled to 25 C, quenched by the addition of dil. aq. hydrochloric acid (2 N, 10 ml), and extracted with ether (3 × 100 ml). The organic phases were dried (Na2SO4), the solvents evaporated, and the crude product subjected to chromatography (silica gel, hexane/ethyl acetate mixtures).

The synthetic route of 25245-35-6 has been constantly updated, and we look forward to future research findings.

Synthetic Route of 116632-41-8, 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. 116632-41-8 name is 2-Chloro-5-iodotoluene, 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.

General procedure: In a Schlenk tube are added 6-azaindole (0.846 mmol), potassium phosphate (1.78 mmol) and CuI(0.042 mmol). The tube is twice evacuated and back-filled with Ar. Toluene (1 ml), 2-chloro-5-iodotoluene (0.846 mmol) and (trans)-N,N’-dimethyl-1,2-cyclohexanediamine (0.085 mmol) are added. The tube is sealed and the reaction mixture is stirred for 22 h at 110 C. The reaction mixture is diluted with dichloromethane and dry loaded on silica gel to be purified by flash chromatography (hexane/EtOAc 10% to 30%) to give 1-(4-chloro-3-methylphenyl)-1H-pyrrolo[2,3-c]pyridine as a white solid (184 mg).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2-Chloro-5-iodotoluene, and friends who are interested can also refer to it.

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. 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Computed Properties of C3H4F3I

To a solution of 500 mg (1.79 mmol) of the compound from Ex. 35A in 22 ml of DMF were added 620 mg (4.49 mmol) of potassium carbonate, and the mixture was stirred at RT for 15 min. Then 1.24 g (5.39 mmol) of 1,1,1-trifluoro-3-iodopropane were added, and the mixture was stirred at 50 C. for 15 h. The DMF was very substantially distilled off and the residue obtained was partitioned between semisaturated sodium chloride solution (100 ml) and ethyl acetate (50 ml). The water phase was extracted with ethyl acetate. The combined organic phases were dried over sodium sulfate, filtered and concentrated. The residue obtained was chromatographed using a silica gel cartridge (Biotage, 100 g of silica gel, eluent: hexane/ethyl acetate 94:6?50:50). In this way, 600 mg (88% of theory) of the title compound were obtained. 1H-NMR (400 MHz, DMSO-d6, delta/ppm): 10.09 (s, 1H), 4.15 (br. d, 2H), 2.85-2.71 (m, 5H), 2.42 (dd, 1H), 1.17 (s, 3H), 1.06 (dd, 1H), 0.87 (s, 3H), 0.73 (dd, 1H). LC/MS (Method 4, ESIpos): Rt=1.32 min, m/z=375 [M+H]+.

The synthetic route of 460-37-7 has been constantly updated, and we look forward to future research findings.

Electric Literature of 35453-19-1, 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. 35453-19-1 name is 5-Amino-2,4,6-triiodoisophthalic acid, 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.

Example 1 Preparation of R iopamidol [R-5-(alpha-hydroxypropionylamino)-2,4,6-triiodoisophthalic add di-(1,3 dihydroxyisopropylamide)]. 400g (0.72 Mole) 5-amino-2,4,6-triiodoisophthalic acid should be added to 200 ml thionyl chloride, the mixture boiled and stirred for six hours, and the resulting solution then evaporated. The residue should then be dissolved in anhydrous ethyl acetate, and the solution should again be evaporated to dryness. The solid material should then be dissolved in 4000 ml ethyl acetate, and the solution stirred into an ice-cold solution of 500 g sodium chloride and 200 g sodium bicarbonate in 2.5 liters water. The organic phase should be separated from the aqueous solution, washed with aqueous sodium chloride solution, dried by contact with anhydrous calcium chloride, and evaporated to dryness. The resulting 5-amino-2,4,6-triiodoisophthalyl chloride has a melting point of about 300C when recrystallized from toluene.

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