Month: April 2021

Application of 2974-94-9, These common heterocyclic compound, 2974-94-9, name is 1-Iodo-4-phenoxybenzene, 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.

Example 2A 3-(4-phenoxyphenoxy)quinuclidine 3-Hydroxy quinuclidine (Aldrich, 254 mg, 2 mmol) was treated with 1-iodo-4-phenoxy-benzene (Aldrich, 296 mg, 1 mmol), Cul (Strem Chemicals, 19 mg, 0.1 mmol), 1,10-phenanthroline (Aldrich, 36 mg, 0.2 mmol), and Cs2CO3 (660 mg, 2.0 mmol) in toluene (anhydrous, Aldrich, 10 mL) and heated at 110 C. for two days. After cooling to room temperature, the reaction mixture was diluted with ethyl acetate (50 mL) and washed with water (2*10 mL). The organic phase was concentrated and the title compound was purified by chromatography (SiO2, CH2Cl2:MeOH:NH3H2O, 90:10:1, Rf. 0.20) as oil (220 mg, yield, 75%). 1H NMR (MeOH-d4, 300 MHz) delta 1.45-1.58 (m, 1H), 1.64-1.85 (m, 2H), 2.00-2.15 (m, 1H), 2.20-2.30 (m, 1H), 2.70-3.10 (m, 5H), 3.34-3.40 (m, 1H), 4.52 (m, 1H), 6.83-6.98 (m, 6H), 7.03 (tt, J=7.5, 1.0 Hz, 1H), 7.20-7.41 (m, 2H) ppm. MS (DCl/NH3) m/z 296 (M+H)+.

Statistics shows that 1-Iodo-4-phenoxybenzene is playing an increasingly important role. we look forward to future research findings about 2974-94-9.

Synthetic Route of 1271523-34-2, A common heterocyclic compound, 1271523-34-2, name is 1,5-Dichloro-2-iodo-3-methoxybenzene, molecular formula is C7H5Cl2IO, 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.

To a solution of 11a (21.0g, 69.3mmol) in THF (250ml) was sequentially added Cul (1.32g, 6.9mmol) and NaH (60% dispersion in mineral oil, 4.2g, 104mmol), followed by a slow addition of pinacolborane (15.1ml, 104mmol). The resulting suspension was stirred at room temperature for 16 h under a N2 atmosphere, and then quenched with saturated NH4CI (250 ml). After 20 min, the mixture was extracted with EtOAc (x3), dried and then filtered over Celite. Concentrated and purification by column chromatography (Si02; EtOAc:PE 0: 1?3:7) to afford the title boronate as a white solid; (15. lg, 72%)NMR (CDC13) 6.87 (IH, d, J 1.6), 6.63 (IH, d, J 1.6), 3.37 (3H, s), 1.32 (12H, s);MS (m/e) No MI observed, Rt 1.17min (QC Method 2)

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: 16355-92-3, name is 1,10-Diiododecane, 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 16355-92-3, Formula: C10H20I2

2,15-hexadecanedione as an aliphatic diketone was synthesized. In a 2 L four-necked flask equipped with a thermometer, mixer and a reflux condenser, 260.3 g (2.0 mol) of ethyl acetoacetate and 500 ml of acetone were fed, stirred and mixed, 61.9 g (1.5 mol) of 97% sodium hydroxide was added and reacted for 15 minutes. Then 197.0 g (0.5 mol) of 1,10-diiododecane was added and the reaction was carried out under reflux for 6 hours. After completion of the reaction, acetone was distilled off by distillation under reduced pressure, neutralized by adding 2N hydrochloric acid, and separation was carried out. The upper layer organic layer was separated and 800 g (2.0 mol) of 10% sodium hydroxide aqueous solution was added and stirred at room temperature for 8 hours to carry out a saponification reaction, 205.8 g (1.1 mol) of 50% sulfuric acid was added, and the mixture was fully refluxed for 3 hours for decarboxylation reaction. After the decarboxylation reaction was completed, the upper organic layer was separated by phase separation and cooled to room temperature to obtain 130.8 g of a pale yellow crystal. A small amount of a part of the obtained crystal product was taken for gas chromatograph measurement. As a result of analyzing the composition of the separated crystals by gas chromatography, the conversion of 1,10-diiododecane was 100%, the purity of 2,15-hexadecanedione was 92%.The yield of 2,15-hexadecanedione based on 1,10-diiododecane was 95%

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1,10-Diiododecane, and friends who are interested can also refer to it.

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.

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.

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.

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.

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.

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.

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.