Month: May 2021

Application of 14452-30-3, A common heterocyclic compound, 14452-30-3, name is 1-(3-Iodophenyl)ethanone, molecular formula is C8H7IO, 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: Aryl halide (1 mmol), phenylacetylene (1.5 mmol), and PNIPAM-co-PPAP/Pd catalyst (0.1 mol% Pd based on Aryl halide) were added into a 10 mL overpressure screw-capped vial equipped with a magnetically stirring bar, and then 1 mL deionized water was added. After the mixture was degassed under argon gas for 10 min, Et3N (3 mmol) was added in, and the solution was stirred at a given temperature for appropriate time. After the reaction was completed and cooled to room temperature, the solution was diluted with deionized water, and extracted with ethyl acetate (3 × 6 mL). The organic phase was washed with brine, dried with MgSO4, and then the solvent was evaporated under reduced pressure. The resulting residue was chromatographed on silica gel (hexane/ethyl acetate) to give pure product which was analyzed by 1H and 13C NMR, and the specific data were shown in Supporting Information.

The synthetic route of 14452-30-3 has been constantly updated, and we look forward to future research findings.

Application of 20691-72-9, 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. 20691-72-9, name is 4-Iodo-2-nitroaniline belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Method b: To a mixture of the 4-iodo-2-nitroaniline (142 mmol) and cesium carbonate (55.5 g, 170 mmol) in 2-butanone (740 mL) was dropwise added a solution of Boc2O (37.8 g, 173 mmol) in 2-butanone (170 mL) and the resulting mixture was stirred at 52 C. for 26 h. The solvent was removed in vacuum, the residue was treated with a mixture of H2O (240 mL) and MeOH (240 mL) and extracted with hexane (3*500 mL). The combined hexane layer was washed with brine (200 mL) and all aqueous layers were reextracted with hexane (300 mL). All combined hexane layers were dried over MgSO4, filtered and the solvent was removed in vacuum to give an orange solid, which was purified by silica gel column chromatography with hexane/EtOAc to give the (4-iodo-2-nitro-phenyl)-carbamic acid tert.-butyl ester as a yellow solid.

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-Iodo-2-nitroaniline, other downstream synthetic routes, hurry up and to see.

Reference of 4949-69-3, A common heterocyclic compound, 4949-69-3, name is 4-Iodo-3-methylaniline, molecular formula is C7H8IN, 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 CuCl (5 g, 50.5 mmol) and pyridine (50 mL) was stirred at r.t. for 30 min. The suspension was filtered and the halogenated aniline (1.5 equiv) was added to the green solution. Air was bubbled through the solution for 18 h. The residue was diluted with CH2Cl2 (200 mL) and aq 1 M HCl (100 mL). The aqueous layer was extracted with CH2Cl2 (3 × 100 mL). The combined organic layers were washed with H2O (100 mL), dried (MgSO4), and concentrated.The crude product was recrystallized from EtOH.

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 16932-44-8, 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. 16932-44-8, name is 2-Iodo-1,3-dimethoxybenzene, This compound has unique chemical properties. The synthetic route is as follows.

Example 15; 1 ) Me3SiCCH,9I (93%)[0125] 2,6-Dimethoxyphenylacetylene (91). To a stirred, degassed solution of 2-iodo-l ,3- dimethoxybenzene (13.2 g, 50 mmol), trans-dichlorobis(triphenylphosphine)palladium(II) (702 mg, 1 mmol), triphenylphospine (524 mg, 2 mmol), and copper(I) iodide (288 mg, 1.5 mmol) in 3 : 1 (v/v) toluene : diisopropylamine (200 mL) under argon is addedtrimethylsilylacetylene (8.0 mL, 57 mmol). The resulting mixture is stirred under argon at room temperature for lh, followed by 48 hour at 60C, during which period a heavy precipitate attributed to iPr2NH»HI is formed. Contents are passed on a Si02 plug with ethyl acetate as eluent. Volatiles are evaporated under reduced pressure, and the contents are passed on a short Si02 column with 95 :5 to 90: 10 pentane : ethyl acetate (v/v) as the eluent to afford the crude TMS-protected alkyne as an off-white solid that is directly carried to the next step without further purification. The solid is dissolved in THF (90 mL) and the solution is degassed by bubbling argon gas through for ca. 30 min. To the stirred mixture is added by a solution of sodium hydroxide (6 g) in methanol (30 mL). The reaction mixture is stirred at room temperature for lh, before pouring of the contents in saturated aqueous NaCl. After extration with diethyl ether and evaporation of the volatiles, the crude alkyne is purified by passage through a short Si02 column using 1 : 1 dichloromethane : pentane (v/v) as the eluent to afford alkyne 91 as a beige solid (7.55 g, 93% over 2 steps). 1H-NMR (CDC13, 300 MHz): delta = 7.25 (t, J = 8.4 Hz, 1H), 6.54 (d, J = 8.4 Hz, 2H), 3.89 (s, 6H), 3.57 (s, 1H). 13C-NMR (CDC13, 75 MHz): delta =161.9, 130.2, 103.2, 99.9, 85.3, 76.3, 55.9. Characterization data for 91 are consistent with literature values (See Wayland, B. B.; Sherry, A. E.; Poszmic, G.; Bunn, A. G. J. Am. Chem. Soc. 1992, 1 14, 1673-1681).

The chemical industry reduces the impact on the environment during synthesis 2-Iodo-1,3-dimethoxybenzene. I believe this compound will play a more active role in future production and life.

Electric Literature of 19094-56-5, A common heterocyclic compound, 19094-56-5, name is 2-Chloro-5-iodobenzoic acid, molecular formula is C7H4ClIO2, 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.

Oxalyl chloride (72 g, 0.56 moles) was added to a slurry of formula 5a (100 g, 0.35 moles) and a catalytic amount of N, N-dimethylformamide (5mL) in fluorobenzene (250 mL) over about 60 minutes at 15-25 C under nitrogen atmosphere. The mixture was stirred at 21-25 C. After completion of the reaction, the reaction mass was concentrated to remove excess oxalyl chloride. The obtained residue was diluted with fluorobenzene (125 mL) and cooled to 15-25 C. Aluminum chloride (53.5 g, 0.40 moles) was added to this reaction mixture portion- wise while keeping the reaction mass temperature below 25 C and maintaining it at same temperature to complete the reaction. After completion of reaction, the reaction mass was quenched into precooled dilute hydrochloric acid (5%, 1700 mL, 0-5 C) at 5-25 C. After stirring for 60 minutes at 20-25 C, the product was extracted with methylene chloride twice (first with 500 mL, then with 250 mL). The combined organic layers were washed with 10% aqueous sodium hydroxide solution (250mL), water (500mL), and 10% aqueous sodium chloride solution (250mL), sequentially. Thereafter, the organic layer was concentrated and the obtained residue was diluted with n-heptane (250mL) and stirred to precipitate formula 7a as a white solid (105 g).

The synthetic route of 19094-56-5 has been constantly updated, and we look forward to future research findings.

Related Products of 391211-97-5, 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. 391211-97-5, name is 3,4-Difluoro-2-((2-fluoro-4-iodophenyl)amino)benzoic acid, This compound has unique chemical properties. The synthetic route is as follows.

Example 3. Preparation of N-((R)-2.3-dihvdroxypropoxy)-3.4-difluoro-2-(2-fluoro-4-iodo-phenylamino)- benzamide (Compound 1) 3,4-Difluoro-2-(2-fluoro-4-iodophenylamino)-benzoic acid (9) (20 g, 0.051 mol) in 100 mL acetonitrile was treated with 1,1′-carbonyldiimidazole (CDI) (8.66 g, 0.053 mol) (Aldrich, Cat No. 11,553-3) and stirred for about 2 hours at 20-25C until the reaction was deemed complete by HPLC (Conditions D). 94 mL (84.9 g) of 9.7% w/w solution of O-{[(4R)-2,2-dimethyl-1,3-dioxolan-4-yl]methyl}hydroxylamine (6) in toluene was then added and stirred for about 4 hours or until the reaction was deemed complete by HPLC (Conditions D). To this mixture was added 66 mL of 5.6 % hydrochloric acid solution, and after stirring, the bottom aqueous phase was discarded. Again 66 mL of 5.6 % hydrochloric acid solution was added to the organic phase and stirred at 20-25C for 12-18 hours or until the reaction was deemed complete by HPLC (Conditions D). The bottom layer was then discarded and the remaining organic layer was concentrated under reduced pressure to remove about 10-20% solvent, and the volume was adjusted to about 9-11 mL/g with toluene (80 mL). Crude product was then crystallized at 10-15C. The slurry was allowed to stir for about 2 hours and the crude solid product was filtered, and dried. The dried crude product was recharged to the reactor and dissolved into 150 mL of 5% v/v ethanol/toluene mixture at 55- 67C. The solution was then clarified at this temperature through filter (line filter) to remove any remaining particulate matter. The solution was then cooled slowly to 5C to crystallize and stirred for at least 2 h, filtered and dried. The dried solid product was redissolved in EtOH (60 mL) at 35C, and product was precipitated out by adding water (300 mL) at 35C followed by cooling to 200C. The slurry was stirred for at least 2 hours to transform the crystals to the desired polymorphic Form IV as determined by DSC and Powder X-ray Diffraction pattern (PXRD). The slurry was filtered and dried under vacuum oven at 70- 90C to yield the final N-((R)-2,3-dihydroxypropoxy)-3,4-difluoro-2-(2-fluoro-4-iodo-phenylamino)- benzamide (Compound I) product. Overall chemical yield was 13 g, 53%. Melting point (DSC): 112+1 C. Appearance: White to off-white crystals.Shown in Figure 1, PXRD conforms to polymorphic crystal Form IV disclosed in the above mentioned U.S. Patent Application No. 10/969,681 EPO 1H NMR (400 MHz, (CD3)2SO): delta 11.89 (bs, 1H), 8.71 (bs, 1H), 7.57 (d, 1H), 7.37 (m, 2H), 7.20 (q, 1H), 6.67 (m, 1H), 4.84 (bs, 1H), 4.60 (m, 1H), 3.87 (m, 1 H), 3.7 (m, 2H), 3.34 (m, 2H).

The chemical industry reduces the impact on the environment during synthesis 3,4-Difluoro-2-((2-fluoro-4-iodophenyl)amino)benzoic acid. I believe this compound will play a more active role in future production and life.

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. 6828-35-9, name is 5-Chloro-2-iodoaniline, A new synthetic method of this compound is introduced below., COA of Formula: C6H5ClIN

General procedure: Using a dried tube, equipped with a magnetic stirrer and a septum, 2-iodoaniline (0.22 g,1.0mmol) was dissolved in DMSO (3mL), and KOt-Bu (0.34 g, 3mmol) was added. Themixture was stirred for 5min, then dithiocarbamate (0.296 g, 1.5mmol) was added. Thereaction mixture was heated at 100C and checked by TLC until the starting material wasfinished. The reaction mixture was cooled down to room temperature and then quenchedwith sat. NH4Cl solution (5mL) and extracted with ethyl acetate (10mL×3), dried overanhydrous Na2SO4 and concentrated under vacuum. The residue was purified by flashcolumn chromatography to afford the desired product (146mg, 82%).

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: 10297-05-9, name is 1-Chloro-4-iodobutane, 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 10297-05-9, Recommanded Product: 10297-05-9

(Step 2) [1-(3-Hydroxypropyl)imidazolidin-2-ylidene] malononitrile (1.00 g, 5.21 mmol) obtained in the Step 1 was dissolved in DMF (10 mL) and the solution was sequentially added with potassium carbonate (1.44 g, 10.4 mmol) and 1-chloro-4-iodobutane (1.27 mL, 10.4 mmol). After stirring at room temperature for 18 hours, the mixture was added with saturated brine and extractd with ethyl acetate. The organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate and the solvent was evaporated under reduced pressure. The residue was washed with diisopropylether to obtain [1-(4-chlorobutyl)-3-(3-hydroxypropyl)imidazolidin-2-ylidene]malononitrile (1.35 g, 91.8percent) as a white solid. 1H NMR (CDCl3, deltappm): 1.80-2.00 (m, 6H), 3.53-3.78 (m, 12H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Chloro-4-iodobutane, 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. 401-81-0, name is 1-Iodo-3-(trifluoromethyl)benzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. category: iodides-buliding-blocks

General procedure: Catalyst 1 (prepared according Ref.15a, 7.1 mg,0.05 mequiv of Pd) was added to a solution of aryl iodide (4 mmol,1.0 equiv), methyl acrylate (0.72 mL, 8 mmol, 2.0 equiv), Et3N (0.67 mL,4.8 mmol, 1.2 equiv) in a mixture of toluene (6.7 mL), DMF (3.3 mL) and H2O(0.1 mL). The reaction mixture was heated at 100 C for 20 h. After coolingto rt, 1 was filtered off under vacuum. The mixture of solvents wasconcentrated under vacuum and the residue was purified by flashchromatographyon silica gel to afford pure alkenes after drying under,vacuum (0.1 mbar).

The synthetic route of 401-81-0 has been constantly updated, and we look forward to future research findings.

204257-72-7, name is Methyl 2-fluoro-4-iodobenzoate, 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. Computed Properties of C8H6FIO2

2-Fluoro-4-(2,2,4,4-tetramethyl-chroman-6-yl-ethynyl)-benzoic acid methyl ester (Compound 29, General Formula 8) Following general procedure F and using 6-ethynyl-2,2,4,4-tetramethylchroman (0.11 g, 0.51 mmol), methyl-2-fluoro-4-iodo-benzoate (Reagent G, 0.14 g, 0.51 mmol), triethyl amine (5 mL), tetrahydrofuran(10 mL), copper(I)iodide(0.030 g, 0.16 mmol) and dichlorobis(triphenylphosphine)palladium(II) (0.110 g, 0.16 mmol) followed by flash column chromatography over silica gel (230-400 mesh) using 5-10% ethyl acetate in hexane as the eluent, the title compound was obtained (0.14 g, 79%). 1H NMR (300 MHz, CDCl3): delta7.82 (t, 1H, J=7.9 Hz), 7.39 (d, 1H, J=1.8 Hz), 7.25-7.16 (m, 3H), 6.69 (d, 1H, J=8.2 Hz), 3.85 (s, 3H), 1.77 (s, 2H), 1.29 (s, 6H), 1.28 (s, 6H).

The synthetic route of 204257-72-7 has been constantly updated, and we look forward to future research findings.