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. 22236-10-8, name is 4-(Difluoromethoxy)aniline, A new synthetic method of this compound is introduced below., Computed Properties of C7H7F2NO

General procedure: N-substituted benzylidene pyrrolidine dione (0.5 mol),0.6 mmol TBTU, and 0.6 mmol EDCI were dissolved in 2mL DCM and 0.75 mmol DIEA mixture solution and stirred for 30 min. Next, 0.5 mol of amine or methylamino acid in DCM (8 mL) solution was slowly added to the solution and stirred at room temperature for 4-10 h with the TLC monitoring reaction. After the reaction was complete, the resultant solution was washed with dilute hydrochloricacid and saturated sodium bicarbonate solution, then dried with anhydrous sodium sulfate, followed by column chromatography separation. The target product was obtained by crystallization.The yield ranged from 72 to 90%.

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.

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. 13940-96-0, name is 4-Phenoxybenzene-1,2-diamine, This compound has unique chemical properties. The synthetic route is as follows., Product Details of 13940-96-0

20 ml of 6N HC1 was added to 1000 mg of 4-phenoxybenzene-l, 2-diamine in round bottom flask. Then add 500 pL of thioglycolicacid. This reaction mixture was refluxed for 4 hours. Excess solvent was evaporated under reduced pressure and to the remaining residue water (30 ml) was added and then extraction with ethyl acetate. The organic solvent was then dried over anhydrous MgS04 and evaporated under reduced pressure. The crude product was directly used in the next step without any further purification. LC.MS: m/z 257.06 (M+H)+.

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 13940-96-0.

Electric Literature of 2688-84-8, These common heterocyclic compound, 2688-84-8, name is 2-Phenoxyaniline, 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 a 1 L round bottom flask reactor 2-Phenoxyaniline (25.0, 0.135 mol), hydrochloric acid (30 ml) and water (150 ml) were added and the mixture was cooled to 0 C and stirred for 1 hour. 75 ml of an aqueous solution of sodium nitrite (11.2 g, 0.162 mol) was added dropwise to the reaction solution at the same temperature, followed by stirring for 1 hour. When 75 ml of an aqueous solution of potassium iodide (44.8 g, 0.270 mol) was added dropwise, the temperature of the reaction solution was dropped so that the temperature did not exceed 5 C. After stirring for 5 hours at room temperature, the reaction mixture was washed with an aqueous solution of sodium cyanosulfate and extracted with ethyl acetate and water. The organic layer was separated and concentrated under reduced pressure, followed by separation and purification by column chromatography to obtain Intermediate 5-a. (22.6 g, 56.5%).

Statistics shows that 2-Phenoxyaniline is playing an increasingly important role. we look forward to future research findings about 2688-84-8.

Electric Literature of 101-84-8, These common heterocyclic compound, 101-84-8, name is Diphenyl oxide, 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.

Comparative Example; A 500 milliliter four-neck round bottom flask was fitted with a mechanical stirrer, a double walled reflux condenser, a thermocouple, a temperature controller, a heating mantle, and a syringe pump fitted with a Teflon needle. The flask was vented to a water trap for collection of by-product hydrogen bromide. Dry bromine (929.5 grams, 5.82 moles, 200% excess) was charged into the reaction flask, followed by 4.1 grams of aluminum chloride (0.031 mole). The reaction was stirred for 5 minutes.Addition of 33.0 grams (0.19 mole) of diphenyl ether was initiated to the bromine-catalyst mixture at a temperature of 25C. The diphenyl ether addition was maintained at a constant rate by use of a syringe pump over a period of about 180 minutes. The reaction temperature was allowed to increase by way of exotherm to about 35C. Additional heat was applied after the diphenyl ether addition had been completed, and the reaction temperature increased to about 59C within about 20 minutes. After 180 minutes of post addition heating, the heat input was removed and the reaction allowed to cool to room temperature in about 90 minutes.A two liter four-neck round bottom flask was fitted with a mechanical stirrer, a distilling head, a double walled reflux condenser, a thermocouple, a temperature controller, and a heating mantle. One liter of water and the reaction slurry were charged to the flask and the excess bromine was distilled off until a temperature of 100C was achieved.Decabromodiphenyl ether was filtered from the aqueous slurry, washed with water, and dried at 100 C. in a forced air oven.Gas chromatographic analysis of the resulting product showed decabromodiphenyl ether 96.93 area percent, nonabromodiphenyl ether isomers totaling 2.79%, octabromodiphenyl ether isomers totaling 0.25%, and heptabromodiphenyl ether isomers totaling 0.02%.; Example 1; A two liter four-neck round bottom flask was fitted with a mechanical stirrer, a double walled reflux condenser, a thermocouple, a temperature controller, a heating mantle, and a syringe pump fitted with a Teflon needle. The flask was vented to a water trap for collection of by-product hydrogen bromide. Dry bromine (3,410 grams, 21.34 moles, 1000% excess) was charged into the reaction flask, followed by 17.9 grams of aluminum chloride (0.13 mole). The reaction was stirred for five minutes.Addition of 33.0 grams (0.19 mole) of diphenyl ether was initiated to the bromine-catalyst mixture at a temperature of 25 C. The diphenyl ether addition was maintained at a constant rate by use of a syringe pump over a period of about 60 minutes. The reaction temperature was allowed to increase by way of exotherm to about 35 C. Additional heat was applied after the diphenyl ether addition had been completed, and the reaction temperature increased to about 59 C. within about 20 minutes. After about 60 minutes of post addition heating, the heat input was removed and the reaction allowed to cool to room temperature in about 90 minutes.A three liter four-neck round bottom flask was fitted with a mechanical stirrer, a distilling head, a double walled reflux condenser, a thermocouple, a temperature controller, and a heating mantle. One liter of water and the reaction slurry were charged to the flask and the excess bromine was distilled off until a temperature of 100 C. was achieved.Decabromodiphenyl ether was filtered from the aqueous slurry, washed with water, and dried at 100 C. in a forced air oven.Gas chromatographic analysis of the resulting product showed decabromodiphenylether 99.95 area percent, nonabromodiphenyl ether isomers totaling 0.05%, with no other isomers present.; Example 2; The procedure of Example 1 was repeated except that the amount of aluminum chloride was reduced to 6.2 grams (0.047 mole).Gas chromatographic analysis of the resulting product showed decabromodiphenylether 99.90 area percent and nonabromodiphenyl ether 0.1%, with no other isomers present.; Example 3; A two liter four-neck round bottom flask was fitted with a mechanical stirrer, a double-walled reflux condenser, a thermocouple, a temperature controller, a heating mantle, and a syringe pump fitted with a Teflon needle. The flask was vented to a water trap for collection of by-product hydrogen bromide. Dry bromine (3410.1 grams, 21.34 moles, 1000% excess) was charged into the reaction flask, followed by 6.5 grams of aluminum chloride (0.049 mole). The reaction was stirred for five minutes.Addition of 33.0 grams (0.19 mole) of diphenyl ether was initiated to the bromine-catalyst mixture at a temperature of 25 C. The diphenyl ether addition was maintained at a constant rate by use of a syringe pump over a period of about 60 minutes. The reaction temperature was allowed to increase by way of exotherm to about 31 C. Additional heat was applied after the diphenyl ether addition had been completed, and the reaction temperature increased to about 59 C. within about 20 minutes. After about 24 hours of post…

The synthetic route of 101-84-8 has been constantly updated, and we look forward to future research findings.

Related Products of 707-07-3, A common heterocyclic compound, 707-07-3, name is (Trimethoxymethyl)benzene, molecular formula is C10H14O3, 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.

l-(2-Chloro-acetyl)-2-oxo-2,3-dihydro-lH-indole-6-carboxylic acid methyl ester (220.0 g / 0.8219 mol) was suspended in toluene (1096.8 ml) at ambient temperature. Acetic anhydride (269.4 ml / 3.49 eq) was added and the mixture stirred at reflux. To the reaction, trimethyl orthobenzoate (339.10 ml / 2.40 eq) was added within one hour and the reaction continued to stir at 104 C for 3.5 hours and than at ambient temperature for 5 days. The reaction was cooled to 0C, stirred for an additional hour and filtered. The solid was washed with toluene, toluene/EtOAc (1 :1) and Et20 and dried under vacuum to isolate 246.6 g (77.8 %) of l-(2-chloro-acetyl)-3-[l-methoxy-l-phenyl-meth-(E)-ylidene]-2-oxo-2,3-dihydro-lH- indole-6-carboxylic acid methyl ester.

The synthetic route of 707-07-3 has been constantly updated, and we look forward to future research findings.

Reference of 710-18-9, 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. 710-18-9, name is 1-Methoxy-4-(trifluoromethoxy)benzene belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

PREPARATION 18 Synthesis of 2-methoxy-5-trifluoromethoxybenzoyl chloride Combine 2-methoxy-5-trifluoromethoxybenzene (1.0 g, 5.2 mmol) and trifluoroacetic acid (200 mL). Add slowly portionwise hexamethylenetetraamine (26 g, 185.7 mmol). Heat at 60 C. After 24 hours, cool to ambient temperature and pour the reaction mixture into a 2 M aqueous solution of sulfuric acid (500 mL). Cool and extract ten times with diethyl ether. Dry the combined organic layers over Na2 SO4, filter, and evaporate in vacuo to give a residue. Chromatograph the residue on silica gel eluding with 1/4 ethyl acetate/hexane to give 2-methoxy-5-trifluoromethoxybenzaldehyde.

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-Methoxy-4-(trifluoromethoxy)benzene, other downstream synthetic routes, hurry up and to see.

Adding a certain compound to certain chemical reactions, such as: 14542-71-3, name is 3,5-Dibromo-4-methylanisole, belongs to ethers-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 14542-71-3, Application In Synthesis of 3,5-Dibromo-4-methylanisole

Step A: 2,6-Dibromo-4-methoxy-benzyl bromide To a suspension of 5.0 g of 2,6-dibromo-4-methoxytoluene in 90 mL of CCl4 was added N-bromosuccinimide and benzoyl peroxide. The resulting mixture was heated to reflux and stirred at the refluxing temperature while irradiating with a sunlamp for 2 h, then cooled and concentrated. The resulting residue was dissolved in 1:1 hexanes-Et2O and filtered through a pad of silica gel, then purified by flash chromatography on a Biotage 40M column, eluding with 98:2 hexanes-Et2O, to yield 2,6-Dibromo-4-methoxy-benzyl bromide as a pale yellow solid. IH NMR (500 MHz, 2,6-Dibromo-4-methoxy-benzyl bromide as a pale yellow solid. 1H NMR (500 MHz,

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3,5-Dibromo-4-methylanisole, and friends who are interested can also refer to it.

148583-65-7, name is 4-Fluoro-2-isopropoxyaniline, belongs to ethers-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. category: ethers-buliding-blocks

Example 54; Lambda/-(3-(Dimethylamino)propyl)-4-(4-fluoro-2-/so-propoxyphenylamino)-5- methylthieno[2,3-c/]pyrimidine-6-sulfonamide; 4-Fluoro-2-/so-propoxyaniline (0.049 g, 0.28 mmol) and 4-chloro-Lambda/-(3- (dimethylamino)propyl)-5-methylthieno[2,3-c/]pyrimidine-6-sulfonamide hydrochloride salt (0.1 g, 0.28 mmol) were heated at 70 0C in anhydrous 1 ,4-dioxane (1.5 ml_) for 4 hours. The solution was cooled to ambient temperature and diluted with water (2.0 ml_) and adjusted to pH 9 (4:1 water/ ammonium hydroxide solution). The precipitate was collected, washed with water and diethyl ether to yield the title compound as beige solid (0.039 g, 28 %).1H NMR (400 MHz; d6-DMSO; 25 C): delta 8.60 (s, 1 H), 8.55-8.50 (m, 1 H), 8.49 (s, 1 H), 8.30 (bs, 1 H), 7.13 (dd, 1 H), 6.87 (dt, 1 H), 4.85-4.80 (m, 1 H), 3.00 (s, 3H), 2.99-2.93 (m, 2H), 2.25 (t, 2H), 2.10 (s, 6H), 1.59-1.55 (m, 2H), 1.35 (d, 6H). MS (ESI+): 482 (M+H). HPLC (10cm_ESI_Formic): Rt 2.41 min (HPLC purity 98 %).

The synthetic route of 148583-65-7 has been constantly updated, and we look forward to future research findings.

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. 16452-01-0, name is 3-Methoxy-4-methylaniline, This compound has unique chemical properties. The synthetic route is as follows., Formula: C8H11NO

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According to the analysis of related databases, 16452-01-0, the application of this compound in the production field has become more and more popular.

Electric Literature of 102503-23-1, 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. 102503-23-1 name is 1-(2,4-Dimethoxyphenyl)-N-methylmethanamine, 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.

b) 1-(2,4-dimethoxyphenyl)-N-methyl-N-[S-methyl-N-(2,2,2-trifluoroethyl)-sulfonimidoyl] methanamineCaution: t-BuOCl is light sensitive (work in a dark hood) and reacts violently with rubber, do not use rubber septum.To a stirring solution of N-(2,2,2-trifluoroethyl)methanesulfinamide (1.5 g, 9.31 mmol, (0249) Eq: 1.00) in dry tetrahydrofurane (THF) (50 ml) at -78 C was quickly added tert-butyl hypochlorite (1.06 g, 1.11 ml, 9.77 mmol, Eq: 1.05) and the mixture was stirred at -78 C for 10 min. 1-(2,4-dimethoxyphenyl)-N-methylmethanamine (2.02 g, 11.2 mmol, Eq: 1.2) (CAS 102503-23-1) in THF (10 ml) were added dropwise to the reaction mixture at -78C followed by triethylamine (1.88 g, 2.59 ml, 18.6 mmol, Eq: 2.0) and stirred at -78 C for 10 min. The cooling bath was replaced by an ice bath and the mixture was stirred at 0 C for 1 h, then at 22 C for 30 min. Saturated aqueous sodium hydrogen carbonate (NaHCO3,-solution was added and stirred at room temperature for 10 min. After that the mixture was poured cautiously into 1N aqueous HCl solution, diluted with ethyl acetate, and the phases were separated. The organic layer was washed with brine, dried over sodium sulfate (Na2SO4), filtered and evaporated to dryness. The crude material was purified by flash chromatography (silica gel, 40 g, 25% to 60% ethyl acetate (EtOAc) in heptane) to yield the title compound as a white solid (2.56 g; 80.8%). MS (ESI): m/z= 341.2 [M+H]+

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-(2,4-Dimethoxyphenyl)-N-methylmethanamine, and friends who are interested can also refer to it.