Month: April 2021

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. 25245-27-6, name is 1-Iodo-3,5-dimethoxybenzene, A new synthetic method of this compound is introduced below., category: iodides-buliding-blocks

To a mixture of 600 mg (4.0 mmol) of 3-methoxyphenylboronic acid, 792 mg (3.0 mmol) of 3,5-dimethoxyiodobenzene, 34 mg (5 mol %) palladium(II)acetate, 182 mg (20 mol %) of tri-o-tolylphosphine, and 3.6 g (24 mmol) of cesium fluoride was added 10 mL of anhydrous dioxane. The reaction was stirred at reflux under N 2 for 50 min, then poured into 30 mL of water and extracted with diethyl ether (3 10 mL). The combined ether layers were back extracted with saturated aqueous NaHCO 3 solution (1 10 mL), then brine (1 10 mL), dried over MgSO 4, filtered, and concentrated to an oil. This was purified via silica gel chromatography, eluting with 10%, ethyl acetate:hexanes to provide the titled compound (650 mg, 89%).

The synthetic route of 25245-27-6 has been constantly updated, and we look forward to future research findings.

Some common heterocyclic compound, 672-57-1, name is 1-Chloro-2-iodo-4-(trifluoromethyl)benzene, molecular formula is C7H3ClF3I, 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. category: iodides-buliding-blocks

Methyl-4-iodosalycilate 1 or 4-Chloro-3-iodobenzotrifluoride 2 (1.00 mmol) and 5-formyl-2-furan boronic acid 3 were dissolved in 10 mL of DMF and 15 mL of EtOH. The reaction mixture was stirred for 10 min under N2, then Pd(PPh3)2Cl2 (0.10 mmol) was added and finally Na2CO3 2M (6.00 mmol). The reaction mixture (light-orange) was stirred under N2 at room temperature. After 1h the reaction went to completion and was quenched with H2O and 2N HCl; then EtOAc was added and the mixture was stirred until the two layers became clear. The aqueous layer was extracted three times with EtOAc, then the organic phase was washed several times with H2O and brine, dried over Na2SO4, filtered and evaporated under reduced pressure. 5-(2-chloro-5-(trifluoromethyl)phenyl)furan-2-carbaldehyde (4). The crude product was purified by flash chromatography using PE/EtOAc = 4:1 as eluent to yield the wished product 4 as a brown solid (yield: 20%); mp = 157 C (decomposition); 1H NMR (400 MHz, CDCl3) delta 9.73 (s, 1H), 8.23 (s, 1H), 7.76-7.45 (m, 2H), 7.42-7.28 (m, 2H)ppm. MS (ESI): m/z 273.0 [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 672-57-1, its application will become more common.

Related Products of 811842-30-5, These common heterocyclic compound, 811842-30-5, name is 2-Bromo-1-fluoro-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.

A mixture of 2-bromo-1-fluoro-4-iodobenzene (3.01 g, 10 mmol), Example 35a (1.472 g, 10.50 mmol), and cesium carbonate (3.42 g, 10.50 mmol) in dimethylsulfoxide (20 mL) was heated at 110 C overnight. After cooling to ambient temperature, the reaction mixture was partitioned between water and ethyl acetate. The aqueous layer was extractedwith additional ethyl acetate twice. The combined organic layers were washed with brine, dried over anhydrous magnesium sulfate, filtered, and concentrated. The residue was purified by column chromatography on silica gel eluting with heptanes to give the title compound (3.21 g, 76% yield) as a white solid.

The synthetic route of 811842-30-5 has been constantly updated, and we look forward to future research findings.

These common heterocyclic compound, 355-43-1, name is 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-6-iodohexane, 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. Recommanded Product: 355-43-1

General procedure: In a Pyrex glass tube were placed TTMSS (0.2 mmol), olefin (0.24 mmol), perfluoroalkyl iodide (0.24 mmol) and CH2Cl2 (5 mL). Then Na2S2O3 (0.5 mmol, 79 mg) and water (1 mL) were added to the mixture. After sealing the tube, the mixture was shaken and then irradiated with a Hg lamp at room temperature. After the reaction was completed, the mixture was extracted with CH2Cl2. The extract was washed with brine, dried over Na2SO4, filtered, and concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography to afford pure product.

The synthetic route of 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-6-iodohexane has been constantly updated, and we look forward to future research findings.

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. 2142-70-3, name is 1-(2-Iodophenyl)ethanone, A new synthetic method of this compound is introduced below., Application In Synthesis of 1-(2-Iodophenyl)ethanone

General procedure: To the mixture of o-bromoacetophenone derivatives 1 (1.0 mmol), t-BuOK (2.0 mmol, 2.0 equiv) and amines 2 (2.0 mmol, 2.0 equiv), dry 1,4-dioxane (5 mL) was added. The mixture was refluxed at 140 C under N2 without light for 16 h. The reaction was monitored by TLC. Then, the resulting reaction mixture was diluted with water (10 mL), eluting with EtOAc (3 * 15 mL). The organic layer was dried over anhydrous Na2SO4 followed by concentration under reduced pressure and purified by column chromatography using petroleum ether/ethyl acetate to afford the corresponding products.

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 351003-36-6, 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 351003-36-6 as follows.

A solution of 2-fluoro-5-iodobenzonitrile (100 mg, 0.405 mmol) and 2-methyl- 2,4-dihydro-3H-pyrazol-3-one (63.6 mg, 0.648 mmol) in 5 ml_ of 1 -methyls- pyrrol id inone was treated with cesium carbonate (396 mg, 1.22 mmol) and stirred at 110 0C for 2 hour. The reaction was diluted with 50 ml_ water and extracted with 2 x 5OmL ethyl acetate. The combined organic layers were washed with 50 ml_ water, 5OmL brine, dried over magnesium sulfate, filtered, and evaporated to afford crude material. Purification by normal phase chromatography provided the title compound as a white solid (93 mg). LC/MS 5-100% acetonithle/tfa-water/tfa (6 min gradient) 4.74 min [(M+H)+ = 326]. 1 H NMR (400 MHz, DMSO- c/6) delta ppm 8.33 (1 H, d, J=2.2 Hz), 8.04 (1 H, dd, J=8.9, 2.2 Hz), 7.45 (1 H, d, J=2.0 Hz), 6.95 (1 H, d, J=8.9 Hz), 5.99 (1 H, d, J=2.0 Hz), 3.67 (3 H, s)

According to the analysis of related databases, 351003-36-6, the application of this compound in the production field has become more and more popular.

Related Products of 627-31-6, 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. 627-31-6 name is 1,3-Diiodopropane(stabilized with Copper chip), 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: K2CO3 (3.7g, 26.8mmol) was added to a solution of 3-(4-hydroxyphenyl)-thiazolidine-2,4-dione (10, 2.8g, 13.4mmol) in MeCN (20mL) and stirred for 10min. The appropriate diiodoalkane (80.3mmol) was added and the reaction mixture was stirred at 95C for 7h. After cooling, water (10mL) was added followed by extraction with ethyl acetate. The organic layer was dried over anhydrous MgSO4, filtered and evaporated under reduced pressure. The residue was purified by flash column chromatography (SiO2, n-hexane/ethyl acetate= 3/1 v/v) to afford the desired compounds.4.1.5 61 3-(4-(3-Iodopropoxy)phenyl)thiazolidine-2,4-dione (11a) (0021) White solid, yield: 81%, 4.0g, 1H NMR (400MHz, DMSO-d6) delta: 2.19-2.24 (m, 2H), 3.39 (t, J=6.6Hz, 2H), 4.06 (t, J=4.7Hz, 2H), 4.28 (s, 2H), 7.05 (d, J=7.1Hz, 2H), 7.20 (d, J=7.1Hz, 2H). HRMS (ES+): m/z calculated for C12H12INO3S: 399.9481 [M+Na]+. Found 399.9472.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1,3-Diiodopropane(stabilized with Copper chip), and friends who are interested can also refer to it.

Adding a certain compound to certain chemical reactions, such as: 167479-01-8, name is tert-Butyl (3-iodopropyl)carbamate, 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 167479-01-8, COA of Formula: C8H16INO2

Compound 7?. A solution of 3-bromo-N-(tert-butoxycarbonyl)propylamine23 (1.61g; 5.66mmol) and cyclen glyoxal (1g; 5.15mmol) in freshly distilled THF (25mL) was stirred at room temperature for 3 days until completion, as monitored by TLC. The white powdery precipitate was filtered and washed with diethylether to afford compound 7? (2.25g; 91% yield). 1H NMR (D2O, 300MHz) delta: 3.99-3.45 (m, 9H), 3.33-3.21 (m, 6H), 2.98-2.79 (m, 5H), 2.63-2.47 (m, 2H), 2.21-2.02 (m, 2H, CH2CHNHBoc), 1.48 (s, 9H, C(CH3)3). 13C NMR (D2O, 75MHz) delta: 160.9 (CO), 86.7 (CHam), 84.2 (C(CH3)3), 74.6 (CHam), 64.9, 59.9, 58.9, 54.1, 51.3, 51.0, 50.6, 50.5, 46.5, 39.9 (CH2NHCO), 30.7 (CH2NHCO), 30.7 (C(CH3)3), 26.3 (CH2CH2NHCO). HRMS (ESI): calculated for C18H34N5O2+ [M]+: 352.27070; found: 352.27067.

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, tert-Butyl (3-iodopropyl)carbamate, other downstream synthetic routes, hurry up and to see.

Reference of 13194-69-9,Some common heterocyclic compound, 13194-69-9, name is 2-Iodo-5-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.

General procedure: A 25mL oven-dried Schlenk tube were added 2-iodoaniline 1a (110mg, 0.5mmol), phenylacetic acid 2a (81.7mg, 0.6mmol) or benzyl chloride 4a (75.9mg, 0.6mmol), selenium powder (118mg, 1.5mmol), CuBr (7.17mg, 10mmol%), KOH (56.1mg, 1.0mmol) or Cs2CO3 (326mg, 1.0mmol), DMSO (1.5mL). The tube was purged with nitrogen three times. Then the reaction mixture was stirred in a preheated oil bath at 120C for 18h. After the reaction was completed, the mixture was diluted with a saturated solution of Na2CO3 (15mL) and extracted with ethyl acetate (3×10mL). The organic layer was dried over anhydrous Na2SO4, then concentrated in vacuo. The residue was purified by silica gel column chromatography (petroleum ether/ethyl acetate, 100/1) to give pure product 3aa.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-Iodo-5-methylaniline, its application will become more common.

Reference 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.

7-PIPSYL-GC (6).; To a suspension of GC (3,99. 8 mg, 0.227 mmol) and 4-iodobenzenesulfonyl chloride (205.7 mg, 0.680 mmol, 3 equiv) in CH2CL2 (2.25 mL) was added pyridine (73 mL, 0.906 mmol, 4 equiv) and the reaction mixture was stirred for 26 h. The solvent was removed under reduced pressure, the residue dissolved in EtOAc and washed with 1M aq. HC1, brine and dried with MGSO4. The crude product was purified by flash column chromatography (gradient 40-99 % EtOAc/hexanes, 1 % AcOH) to obtain 113.8 mg of pure 6 (73% yield) and 24.3 mg of recovered GC (25 %). 1H-NMR (400 MHz, DMSO-d6) 8 8.18-8. 10 (m, 2HA), 7.78-7. 70 (m, 2H), 7.57 (d, J = 5. 5 Hz, 1H, 10- H), 6.52 (s, 1H, 3-OH), 6.13 (s, 1H, 12-H), 5.30 (d, J = 4.2 Hz, 1H, 1-OH), 5.16 (D, J = 4.1 Hz, 1H, 6-H), 5.01 (d, J = 5.5 Hz, 1H, 10-H), 4.85 (dd, J = 12.4, 4.1 Hz, 1H, 7-H), 4. 60 (d, J = 6.5 Hz, 1H, 2-H), 4.09 (dd, J = 6.5, 4.2 Hz, 1H, 1-H), 2.80 (q, J = 7.1 Hz, 1H, 14-H), 1.95 (d, J = 12.4 Hz, 1H, 8- H), 1.10 (d, J = 7.1 Hz, 3H, 16-CH3), 0.98 (s, 9H, tBu) ; 13C- NMR (75 MHz, MEOD) 5 8.16, 29.24, 33.20, 43.17, 50.03, 64.78, 68.71, 70.24, 75.03, 76.67, 81.10, 84.50, 93.47, 100.06, 103.62, 111.14, 130.49, 137.04, 140.39, 171.66, 174.40, 178.05. HRMS (FAB) calcd for C26H28013SI 707.0295, found 707.0265.

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