Tag: M.W=200-300

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.

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.

Related Products of 83863-33-6,Some common heterocyclic compound, 83863-33-6, name is 5-Iodo-2-methylaniline, molecular formula is C7H8IN, 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.

solution of 5-iodo-2-methyl-phenylamine (20.4 g, 87.6 mmol) in 200 mL of dry CH2Cl2 was cooled to 0 C and acetic anhydride (16.5 mL, 175 mmol) was added dropwise. The mixture was heated to 50 C for 2 h and then cooled to 22 C. The resulting white precipitate was filtered to give c (18.4 g, 76%): MS m/z = 276 (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 5-Iodo-2-methylaniline, its application will become more common.

Electric Literature of 90347-66-3, 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. 90347-66-3, name is Methyl 3-iodo-4-methylbenzoate, This compound has unique chemical properties. The synthetic route is as follows.

A suspension of 4-methylimidazole (1, 3.0 g, 36 mmol), 2 (4.8 g, 20 mmol), K2CO3(4.5 g, 33 mmol), CuI (1.14 g, 6 mmol) and 8-hydroxyquinoline (0.56 g, 4 mmol) in DMSO(20 mL) was heated at 120 C overnight under nitrogen. After cooling, water was added andthe mixture was extracted with EtOAc twice. The combined organic layers were washed withbrine, dried over Na2SO4 and concentrated. The residue was purified by silica gel columnchromatography to give 3 (2.8 g, 58%) as a yellow solid. LCMS (m/z: m+1): 242.2. A mixtureof 4 (7.26 g, 26.3 mmol), 5 (3.0 g, 17.5 mmol), K2CO3 (4.84 g, 35.0 mmol), DMEDA (386 mg,4.38 mmol) and CuI (834 mg, 0.871 mmol) in 90 ml of dioxane was stirred at 100 C under N2for 18h. The mixture was filtered, concentrated and purified by column chromatography to give6 (2.2 g, 39%) as a slightly yellow solid. LCMS (m/z: m+1): 320.2. To a solution of 6 (2.2 g,6.89 mmol) in THF/water (60/30 mL) was added LiOH (496 mg, 20.7 mmol). The reactionwas stirred at room temperature overnight, concentrated. To the residue water (30 ml) wasadded and then acidified to pH 4 with aqueous KHSO4. The precipitate was filtered and washedwith water and EtOAc. The cake was collected and dried to give 7 (1.4 g, 67%) as a whitesolid. LCMS: m/z: (M+1): 306. To a solution of 7 (100 mg, 0.33 mmol) in NMP (2 mL) wasadded SOCl2 (58 mg, 0.49 mmol). The reaction was heated at 90 C for 1 hour before 3 (80mg, 0.33 mmol) was added. The resulting mixture was stirred at 90 C for 3 hours. The reactionwas quenched with water and basified with aqueous NaOH. The mixture was extracted withEtOAc twice. The combined organic layers were washed with brine, dried over Na2SO4 andconcentrated. The residue was purified by reverse prep-HPLC and then silica gel prep-TLC togive 1a (22 mg, 13%) as a white solid.

The chemical industry reduces the impact on the environment during synthesis Methyl 3-iodo-4-methylbenzoate. I believe this compound will play a more active role in future production and life.

Adding a certain compound to certain chemical reactions, such as: 61272-76-2, name is 4-Fluoro-2-iodoaniline, 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 61272-76-2, name: 4-Fluoro-2-iodoaniline

General procedure: A mixture of 2-iodoaniline (0.5 mmol), isothiocyanate (0.6 mmol), CuO nanoparticles (0.05 mmol), and Cs2CO3 (1.5 mmol) in PEG-400 (3mL) was stirred at 80°C for 8h (Scheme 1). After the reaction, the reaction mixture was centrifuged and catalyst was separated from the reaction mixture and then followed by washing with ethyl acetate and acetone, dried in vacuo and used directly for further catalytic reactions. The cooled solution was partitioned between ethyl acetate and water, and the organic layer was washed with water and brine, and then dried over Na2SO4. After the removal of the solvent in vacuo, the residue was purified by silica-gel chromatography to give the desired N-substituted-2-aminobenzothiazoles. All the compounds were characterized by comparison with authentic samples [41].

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

Adding a certain compound to certain chemical reactions, such as: 6828-35-9, name is 5-Chloro-2-iodoaniline, 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 6828-35-9, Recommanded Product: 6828-35-9

To a round-bottomed flask charged with 5-chloro-2-iodoaniline (1 g, 3.95 mmol, 1 equiv) was added a solution of 1:1 pyridine in CH2Cl2 (0.7 M, 40 mL) and the reaction mixture was cooled to 0 C. 4-Methylbenzenesulfonyl chloride (750 mg, 3.95 mmol, 1 equiv) was added portionwise, and the reaction mixture was allowed to slowly warm to room temperature and then stirred for 24 h. Upon completion of the reaction, water (80 mL) and CH2Cl2 (80 mL) were added. The reaction mixture was separated and the organics were washed with 1 N NaOH (2 × 40 mL), 1 N HCl (2×40 mL), and brine (2 × 40 mL). The organics were then passed through a hydrophobic frit and concentrated under reduced pressure to give a crude residue, which was purified by flash chromatography (silica gel, 0-12% EtOAc in petroleum ether) to afford the title compound as an off white solid (890 mg, 52%).1H NMR (CDCl3, 500 MHz): delta 7.72-7.65 (m, 3H), 7.57 (d, J = 8.5 Hz, 1H), 7.27 (d, J = 8.0 Hz, 2H), 6.88-6.80 (m, 2H), 2.42 (s, 3H).13C NMR (CDCl3, 126 MHz): delta 144.1, 139.1, 138.1, 135.1, 135.1, 129.4, 127.0, 126.4, 121.4, 88.3, 21.2. Characterisation data is consistent with literature reported values.4

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

Related Products of 4949-69-3, These common heterocyclic compound, 4949-69-3, name is 4-Iodo-3-methylaniline, 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.

3-Thiophenecarboxylic acid (2.0 g, 15.6 mmol) was dissolved in methylene chloride (100 rnL) and 2 drops of DMF were added. The mixture was cooled to about 0 0C and oxalyl chloride (1.5 mL, 17.1 mmol) was added slowly and allowed to warm to room temperature. Gas evolution was observed during warming. 3-Methyl-4-iodoaniline (5.45 g, 23.5 mmol), 4 drops of pyridine and K2CO3 (2.58 g, 18.7 mmol) are dissolved in CH2Cl2 (10 mL) and cooled to about 0 0C. After about Ih, the acid chloride mixture is slowly added to the cooled aniline mixture and allowed to warm to room temperature and stirred for about 18h. The resulting mixture is filtered, washed with ethyl acetate and the filtrate is concentrated to a brown oil. The crude material was purified via flash chromatography (10-30% ethyl acetate in hexanes) to afford the desired product (1.56 g, 29%) as an off-white solid.

The synthetic route of 4949-69-3 has been constantly updated, and we look forward to future research findings.

Electric Literature of 444-29-1, A common heterocyclic compound, 444-29-1, name is 1-Iodo-2-(trifluoromethyl)benzene, molecular formula is C7H4F3I, 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 Schlenk tube was charged with MCM-41-Sb,Py-CuI (122mg, 0.05mmol), triphenyphosphine (26mg, 0.10mmol), and K2CO3 (276mg, 2.0mmol). The tube was evacuated and backfilled with argon. Then, aryl halide (1.0mmol), terminal alkyne (1.2mmol) and DMF (4mL) were added under argon. The tube was sealed, and the reaction mixture was stirred at 100C for 6-24h. The reaction mixture was cooled to room temperature, diluted with ethyl acetate (20mL), and filtered. The MCM-41-Sb,Py-CuI complex was washed with distilled water (2×5mL), DMF (2×5mL), and ethanol (2×5mL) and reused in the next run. The filtrate was washed with water, dried over MgSO4 and concentrated under reduced pressure. The residue was purified by flash column chromatography on silica gel (petroleum/ethyl acetate=30:1-60:1) to provide the desired product.

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.

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. 13194-68-8, name is 4-Iodo-2-methylaniline, A new synthetic method of this compound is introduced below., category: iodides-buliding-blocks

(a) Preparation of 4Fluoro-2-(4iodo-2-methyl-phenylamino)-benzoic acid To a stirred solution containing 3.16 g (0.0133 mol) of 2-amino-5-iodotoluene in 5 mL of tetrahydrofuran at -78 C. was added 10 mL (0.020 mol) of a 2.0 M lithium diisopropylamide in tetrahydrofuran/heptane/ethylbenzene (Aldrich) solution. The resulting green suspension was stirred vigorously for 15 minutes, after which time a solution of 1.00 g (0.00632 mol) of 2,4-difluorobenzoic acid in 10 mL of tetrahydrofuran was added. The reaction temperature was allowed to increase slowly to room temperature, at which temperature the mixture was stirred for 2 days. The reaction mixture was concentrated by evaporation of the solvent under reduced pressure. Aqueous HCI (10%) was added to the concentrate, and the solution was extracted with dichloromethane. The organic phase was dried (MgSO4) and then concentrated over a steambath to low volume (10 mL) and cooled to room temperature. The off-white fibers which formed were collected by vacuum filtration, rinsed with hexane, and dried in a vacuum-oven (76 C.; ca. 10 mm of Hg) to afford 1.10 g (47%) of the desired material; mp 224-229.5 C.; 1H NMR (400 MHz, DMSO): delta 9.72 (s, 1H), 7.97 (dd, 1H, J=7.0, 8.7 Hz), 7.70 (d, 1H, J=1.5 Hz), 7.57 (dd, 1H,.J=8.4, 1.9 Hz), 7.17 (d, 1H, J=8.2 Hz), 6.61-6.53 (m, 2H), 2.18 (s, 3H); 13C NMR (100 MHz, DMSO): delta 169.87, 166.36 (d, JC-F=249.4 Hz), 150.11 (d, JC-F=11.4 Hz), 139.83, 138.49, 136.07, 135.26 (d, JC-F=11.5 Hz), 135.07, 125.60, 109.32, 104.98 (d, JC-F=21.1 Hz), 99.54 (d, JC-F=26.0 Hz), 89.43, 17.52; 19F NMR (376 MHz, DMSO): delta104.00 to -104.07 (m); IR (KBr) 1670 (C=O stretch)cm-1; MS (CI) M+1=372.

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.

Related Products of 54413-93-3, 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. 54413-93-3, name is 2-Iodo-5-methoxybenzoic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

1) Synthesis of 5-methoxy-2-(2H-1 ,2,3-triazol-2-yl)benzoic acid2-lodo-5-methoxy benzoic acid (15.0 g; 53.9 mmol) is dissolved in anhydrous DMF (45 ml) followed by the addition of 1 H-1 ,2,3-triazole (7.452 g; 108 mmol) and cesium carbonate (35.155 g; 108 mmol). By the addition of cesium carbonate the temperature of the reaction mixture increases to 40°C and gas evolved from the reaction mixture. Copper(l)iodide (514 mg; 2.7 mmol) is added. This triggers a strongly exothermic reaction and the temperature of the reaction mixture reaches 70°C within a few seconds. Stirring is continued for 30 minutes. Then the DMF is evaporated under reduced pressure followed by the addition of water (170 ml) and EtOAc (90 ml). The mixture is vigorously stirred and by the addition of citric acidmonohydrate the pH is adjusted to 3-4. The precipitate is filtered off and washed with water and EtOAc and discarded. The filtrate is poured into a separation funnel and the phases are separated. The water phase is extracted again with EtOAc. The combined organic layers are dried over MgS04, filtered and the solvent is evaporated to give 7.1 g of 5-methoxy-2-(2H- 1 ,2,3-triazol-2-yl)benzoic acid as a white powder of 94percent purity (6 percent impurity is the regioisomerically N1-linked triazolo-derivative); tR [min] = 0.60; [M+H]+ = 220.21

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, 2-Iodo-5-methoxybenzoic acid, other downstream synthetic routes, hurry up and to see.