Category: iodides-buliding-blocks

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. 82998-57-0, name is 3-Iodo-4-methylbenzoic acid, This compound has unique chemical properties. The synthetic route is as follows., Safety of 3-Iodo-4-methylbenzoic acid

Add 2 drops of DMF into 628 mg 3-iodo-4-methylbenzoic acid (2.2 mmol) in 20 mL SOCl2 and reflux for 2 h. After vacuum evaporation of SOCl2, add 6.0 mL anhydrous THF and get the pale yellow solution. Dissolve the product from step 1, 524 mg 5-(4-methyl-1H-imidazol-1-yl)-3-(trifluoromethyl)-benzenamine (2.0 mmol) in 6.0 mL anhydrous THF and add 10 mmol Et3N, and the pale yellow solution prepared previously is added drop wise till it is all added. The reaction mixture rises to room temperature for 1 hr. The reaction was quenched with addition of brine and extracted with EtOAc. The combined extraction organic layers was dried and concentrated under vacuum, the residue was purified through column chromatography to afford 873 mg desired product. (90%)MS (ESI), m/z: 486 (M+ + H+).

According to the analysis of related databases, 82998-57-0, the application of this compound in the production field has become more and more popular.

Electric Literature of 13194-68-8, 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. 13194-68-8, name is 4-Iodo-2-methylaniline, This compound has unique chemical properties. The synthetic route is as follows.

A mixture of 1-ethynyl-2-methyl-benzene (70 mg, 602.62 mumol, 75.92 muL, 1 eq), 4-iodo-2-methyl-aniline (140.44 mg, 602.62 mumol, 1 eq), CuI (22.95 mg, 120.52 mumol, 0.2 eq), Pd(PPh3)4 (69.64 mg, 60.26 mumol, 0.1 eq) and butan-1-amine (132.23 mg, 1.81 mmol, 178.68 uL, 3 eq) in THF (5 mL) was degassed and purged with N2 for 3 times. The mixture was stirred at 20 C. for 16 h under N2. The reaction mixture was quenched by addition of water (50 mL), extracted with EtOAc (30 mL*3). The combined organic layers were washed with brine (10 mL), dried over Na2SO4, filtered and concentrated under reduced pressure to give a residue which was purified by flash silica gel chromatography (from PE/EtOAc=1/0 to 5/1, TLC: PE/EtOAc=5/1, Rf=0.23) to yield 2-methyl-4-[2-(o-tolyl)ethynyl]aniline (100 mg, 451.88 mumol, 75.0% yield, 100% purity) as a yellow solid. 1H NMR (400 MHz, CDCl3) delta ppm 7.50-7.43 (m, 1H), 7.27-7.12 (m, 5H), 6.65 (d, J=8.2 Hz, 1H), 3.78 (s, 2H), 2.51 (s, 3H), 2.18 (s, 3H); ES-LCMS m/z 222.2 [M+H]+.

The chemical industry reduces the impact on the environment during synthesis 4-Iodo-2-methylaniline. I believe this compound will play a more active role in future production and life.

Electric Literature of 98-61-3, 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. 98-61-3, name is 4-Iodobenzenesulfonyl chloride belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

5.1.16 4-((4-Iodophenylsulfonamido)methyl)-N-(pyridin-3-yl)benzamide (28) A mixture of amine 27 (727 mg, 3.2 mmol) and 4-iodobenzenesulfonyl chloride (970 mg, 3.2 mmol) in dry pyridine (10 mL) was stirred at 20 C for 16 h. The solvent was evaporated and the residue stirred in water (20 mL) for 1 h. The precipitate was filtered, washed with water (5 mL) and dried. The crude solid was purified by column chromatography, eluting with a gradient (0-20%) of MeOH/EtOAc, to give benzamide 28 (1.47 g, 93%) as a cream powder: mp (MeOH/EtOAc) 249-251 C; 1H NMR delta 10.36 (s, 1H, NHCO), 8.93 (d, J = 2.3 Hz, 1H, H-2′), 8.34 (br s, 1H, NHSO2), 8.31 (dd, J = 4.7, 1.5 Hz, 1H, H-6′), 8.18 (ddd, J = 8.3, 2.5, 1.5 Hz, 1H, H-4′), 7.97 (ddd, J = 8.6, 2.2, 1.9 Hz, 2H, H-2″, H-6″), 7.90 (br d, J = 8.3 Hz, 2H, H-2, H-6), 7.56 (ddd, J = 8.6, 2.2, 1.9 Hz, 2H, H-3″, H-5″), 7.37-7.42 (m, 3H, H-3, H-5, H-5′), 4.09 (s, 2H, CH2N); 13C NMR delta 165.5, 144.5, 142.0, 141.6, 140.3, 138.1 (2), 135.8, 133.1, 128.2 (2), 127.7 (2), 127.5 (2), 127.3, 123.5, 100.3, 45.7; MS m/z 494.6 (MH+, 100%). Anal. Calcd for C19H16IN3O3S: C, 46.26; H, 3.27; N, 8.52. Found: C, 46.43; H, 3.30; N, 8.52.

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

Electric Literature of 391211-97-5, These common heterocyclic compound, 391211-97-5, name is 3,4-Difluoro-2-((2-fluoro-4-iodophenyl)amino)benzoic acid, 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.

In an oven-dried three-neck, 2 L flask was taken 3, 4-DUFLUORO-2- [ (2- fluoro-4-iodophenyl) amino] benzoic acid (196.7g, 0.5 moles) and DMF (900 mL). To this stirred solution was added pyridine (44.4 mL, 43.5g, 0.55 moles) at RT, and then pentafluorophenyl trifluoroacetate (95 mL, 154g, 0.55 moles) was added dropwise within 30 minutes. The mixture was stirred at RT for 20 hours. The mixture was diluted with hexanes-diethyl ether (1 : 1, v/v, 3L) and washed successively with water (2x2L), 1M HC1 (2x2L), saturated NAHCO3 solution (2x2L) and finally with water (2x2L). The organic layer was dried and concentrated under reduced pressure to afford 2,3, 4,5, 6-pentafluorophenyl-3,4- difluoro-2- [ (2-fluoro-4-iodophenyl) amino] benzoate as a red oil (92.3%, 258.5g).

The synthetic route of 391211-97-5 has been constantly updated, and we look forward to future research findings.

Application of 620621-48-9, 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 620621-48-9 as follows.

Example 107 2-Chloro-N-(1 -hydroxy-cyclohexylmethyl)-5-(pyridin-3-yloxy)- benzamide107.1 2-chloro-5-(Dyridin-3-yloxy)benzoic acid methyl esterA microwave vial was charged with copper (I) bromide (7.7 mg), Cs2C03 (685 mg), 3- hydroxypyridine (100 mg) and methyl-2-chloro-5-iodobenzoate (374 mg) and flushed with argon. DMSO (1.6 mL) was added followed by 2-pyridyl acetone (0.014 mL) and the reaction mixture was heated to 100C for 3h in the microwave. It was diluted with EtOAc, filtered and the filtrate was washed with H20. The organic phase was dried over MgS04 and concentrated in vacuo. The crude was purified by CC (Hept/EtOAc 1/0 to 1/1 ) to give 58 mg of the titled compound as a yellowish waxy solid.LC-MS (B): tR = 0.59 min; [M+H]+: 264.26

According to the analysis of related databases, 620621-48-9, the application of this compound in the production field has become more and more popular.

Related Products of 34270-90-1, A common heterocyclic compound, 34270-90-1, name is 1-Iodo-2-(2-iodoethoxy)ethane, molecular formula is C4H8I2O, 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.

Spiro[4H-pyran-4,10′(4’H)-[6H]pyrimido[2,1-c][1,4]thiazepine]-2′-carboxylic acid, 2,3,5,6,7′,8′-hexahydro-3′-hydroxy-4′-oxo-, ethyl ester, 9′,9′-dioxide: To a stirred yellow mixture of intermediate 19/24 (0.1942 g, 0.50 mmol) intermediate 18 (0.208 g, 0.62 mmol) in DMF (5 mL) wad added Cs2CO3 (0.332 g, 1.02 mmol) at once at room temperature. After 24 h, the reaction mixture was diluted with Et2O (50 mL), washed with water (2×10 mL), brine (10 mL), dried (Na2SO4), filtered and concentrated to give colorless paste which was used in the subsequent step without purification.

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 444-29-1, The chemical industry reduces the impact on the environment during synthesis 444-29-1, name is 1-Iodo-2-(trifluoromethyl)benzene, I believe this compound will play a more active role in future production and life.

General procedure: A 10 mL flask equipped with a Teflon valve was charged with a magnetic stir bar, CuI (2 mg, 1molpercent), Heteroarylamine (1.5 mmol), KOtBu (224 mg, 2.0 mmol), solid aryl halides (1.0 mmol). The tube was evacuated and backfilled with argon. Under a counter flow of argon, dioxane (1.5mL), aryl halides (1.0 mmol, if liquid) were added by syringe. The tube was sealed. The reaction mixture was allowed to stir at 110 °C (X=I) or 130 °C (X= Br) for 24 h. Then the mixture was cooled to room temperature and added 5.0 mL brine. Subsequently, the mixture was extracted with ethyl acetate. The organic layers were collected, dried over Na2SO4, filtered and the solvent was removed under vacuum. The residue was purified by column chromatography on silica gel.

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-2-(trifluoromethyl)benzene, other downstream synthetic routes, hurry up and to see.

Adding a certain compound to certain chemical reactions, such as: 25309-64-2, name is 1-Ethyl-4-iodobenzene, 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 25309-64-2, name: 1-Ethyl-4-iodobenzene

General procedure: A 100 mL Schlenk flask was charged with 2-bromopyridine (1.1 mmol), phenylacetylene (0.92 mmol), Cs2CO3 (1.84 mmol), 1-Pd (0.003 mmol based on Pd), DMF (6 mL) and the reaction mixture was stirred at 100 C under air atmosphere for 12 h. The mixture was cooled to the room temperature; the solid was removed by filtration and washed twice with DMF (3 mL). The filtrate was collected, dried and the residue was extracted with ethyl acetate (3 x 3 mL) followed by purification with silica gel chromatography (petroleum ether) to give a corresponding 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-Ethyl-4-iodobenzene, other downstream synthetic routes, hurry up and to see.

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. 628-21-7, name is 1,4-Diiodobutane, A new synthetic method of this compound is introduced below., COA of Formula: C4H8I2

A12 (50.0 mg, 244.82 mumol), 1,4-diiodobutane (48 muL, 367.23 mumol), potassium carbonate (50.8 mg, 367.23 mumol), and anhydrous N, N-dimethylformamide (3 mL) It was added to a 10 mL eggplan60t-shaped flask and stirred at 60 C for 4 hours. After the reaction was detected by TLC, it was filtered and the filtrate was concentrated. After recrystallization (petroleum ether / ethyl acetate, volume ratio of 1: 1), 60.0 mg of white solid was obtained with a yield of 95%. mp: 100-102 C;

The synthetic route of 628-21-7 has been constantly updated, and we look forward to future research findings.

Synthetic Route of 443-85-6, 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. 443-85-6 name is 1-Fluoro-3-iodo-2-methylbenzene, 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.

To a flame dried RBF was added a solution of n-butyllithium (2.5M in hexanes; 3.01 ml, 7.51 mmol) and diethyl ether (15 ml). The solution was cooled to -78 C, and 2- fluoro-6-iodotoluene (0.981 ml, 7.51 mmol) was added dropwise and the reaction was stirred at -78 C for 10 minutes. A -78 C premixed solution of 4-(difluoromethyl)-2-oxa- 3-azabicyclo[3.1.0]hex-3-ene (1.00 g, 7.51 mmol) and boron trifluoride diethyl etherate (0.927 ml, 7.51 mmol) in toluene (10 ml) was added to the reaction via syringe. The reaction was stirred at -78 C for 10 minutes, quenched with saturated ammonium chloride and warmed to RT. The reaction was diluted with water and EtOAc. The organic layer was separated and concentrated under reduced pressure. The crude residue was purified via silica gel flash chromatography eluting with 0-20% ethyl acetate in hexanes to afford 4-(difluoromethyl)-4-(3-fluoro-2-methylphenyl)-2-oxa-3- azabicyclo[3.1.0]hexane (0.81 g, 3.33 mmol, 44.3 % yield). LC/MS (ESI+) m/z = 244.1 (M+H)

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Fluoro-3-iodo-2-methylbenzene, and friends who are interested can also refer to it.