Month: April 2021

592-55-2, name is 1-Bromo-2-ethoxyethane, 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. COA of Formula: C4H9BrO

A mixture of (S)-2-({2-[3-(3-hydroxy-phenyl)-propylamino]-4,6-dimethyl-pyrimidine-5- carbonyl}-amino)-3-[(thiophene-2-carbonyl)-amino]-propionic acid (0.20g, 0.40mmol), 2- bromoethyl ethyl ether (0.3 lg, 2.0mmol), sodium iodide (0.30g, 2.0mmol) and triethylamine (0.20g, 2.0 mmol) in DMF (2.5ml) was microwaved at 120C for 20 minutes. The mixture was diluted with EtOAc, washed with brine, dried over Na2S04, filtered, concentrated in the presence of silica gel and chromatographed (30-100% EtOAc in hexane) to give the title compound (124. lmg, 54% yield). MS m/e 570.2 (M+H+).

The synthetic route of 592-55-2 has been constantly updated, and we look forward to future research findings.

Adding a certain compound to certain chemical reactions, such as: 82830-49-7, name is 2-Fluoro-1,4-dimethoxybenzene, 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 82830-49-7, HPLC of Formula: C8H9FO2

EXAMPLE SIXTY-THREE: General Procedure for Iodoaryl Ligand Precursor; General procedure for the synthesis of B, C, D, and E. An oven-dried three-neck round bottom flask, which was equipped with a magnetic stir bar and charged with magnesium shavings (2.4 equiv), was fitted with a reflux condenser, glass stopper, and rubber septum. The flask was purged with argon and then THF (1 mL/mmol) and the bromo arene (2 equiv) were added via syringe. The reaction mixture was heated to reflux and 1 ,2-dibromethane (40 uL) was added via syringe. The reaction was allowed to stir at reflux for 1.5 h and was then cooled to room temperature. A separate oven-dried round bottom flask, which was equipped with a magnetic stir bar and fitted with a septum, was purged with argon and then THF (10 mL/mmol) and 1 ,4-dimethoxy-2-fluorobenzene (1 equiv) were added to the flask via syringe. The reaction mixture was cooled to -78 0C and n-BuLi (1.05 equiv) was added in a dropwise fashion over a 40 min period. The solution was stirred for 1 h and the Grignard reagent, which was prepared in the first reaction vessel, was added via cannula over a 30 min period and allowed to stir at -78 0C for 1 h. The reaction mixture was warmed to room temperature slowly where it was stirred for an additional 12 h. The mixture was then cooled to 0 0C and a solution of Iodine in THF (I M, 2 equiv) was added via syringe over a 15 min period and then the dark red solution was warmed to room temperature and stirred for 1 h. The solvent was removed via a rotary evaporator, and the remaining dark brown oil was taken up in Et2O, washed with a saturated solution of sodium sulfite, and washed with brine. The organic layer was then dried over MgSO4, filtered, and the solvent was removed via rotary evaporator. The crude material was recrystallized to give the desired product.

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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. 589-10-6, name is (2-Bromoethoxy)benzene, A new synthetic method of this compound is introduced below., Quality Control of (2-Bromoethoxy)benzene

4-hydroxy-1-indanone 1a (5 g, 33.78 mmol)Dissolved in 70 mL of acetonitrile,Potassium carbonate (8 g, 57.9 mmol)Phenoxyethyl bromide (8 g, 40 mmol) was added dropwise,85 stirring reaction 4h, the reaction is complete,The reaction solution was cooled to roomTemperature, filtration, concentration of filtrate under reduced pressure,Get black oil,And then dissolved in 100 mL of ethyl acetate, dried and dried, and purified by column chromatography (petroleum ether: ethyl acetate = 10: 1) to obtain intermediate product 1b(6.39 g, 23.85 mmol,White solid, the yield of 70.6%), directly into the next step.

The synthetic route of 589-10-6 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. 19056-41-8, name is 3-Bromo-4-methoxyaniline, A new synthetic method of this compound is introduced below., Application In Synthesis of 3-Bromo-4-methoxyaniline

Step b: 1-(Benzo[d][1,3]dioxol-5-yl)-N-(3-bromo-4-methoxyphenyl)-cyclopropane-carboxamide (B-10) To a Solution of the Crude 1-Benzo[1,3]Dioxol-5-yl-Cyclopropanecarbonyl Chloride (3.0 mmol) in CH2Cl2 (30 mL) at ambient temperature was added a solution of 3-bromo-4-methoxybenzenamine (3.3 mmol), Et3N (15 mmol), and CH2Cl2 (90 mL) dropwise. The mixture was allowed to stir for 16 h before it was diluted with CH2Cl2 (500 mL). The solution was washed with 1N HCl (2*250 mL), sat. aq. NaHCO3 (2*250 mL), then brine (250 mL). The organics were dried over Na2SO4, filtered, and concentrated in vacuo to provide 1-(benzo[d][1,3]dioxol-5-yl)-N-(3-bromo-4-methoxyphenyl)cyclopropanecarboxamide (B-10) with suitable purity to be used without further purification. Table 4 lists additional N-bromophenyl amides prepared according to preparation 9 and using appropriate starting materials.

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 450-91-9, These common heterocyclic compound, 450-91-9, name is 4-Fluoro-2-methoxyaniline, 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.

Step b: Compound 1a2 (8.0 g, 43 mmol) was added into a 500 ml reaction flask, and concentrated sulfuric acid (100 ml) was added to dissolve the substrate under constant agitation. At -20 C., concentrated nitric acid (6.15 ml, 48 mmol) was slowly added dropwise with stirring, and the reaction mixture was stirred for 5 mins at this temperature. The reaction progress was monitored by TLC. After completion of the reaction, the mixture was poured into ice water. Sodium hydroxide/water solution (150 ml/300 ml) were added slowly to the reaction system at -20 C. in an ice-water bath, and the mixture was adjusted to pH 8-9. The reaction solution was extracted with EA/water system for three times, the organic layer was separated, washed with water, saturated brine, dried over anhydrous Na2SO4, and concentrated under reduced pressure to give compound 1a (8.7 g) which was used directly in the next reaction. Yield: 80%; purity: 100%; MS m/z (ESI): 187.0 [M+H]+; 1H NMR (400 MHz, DMSO-d6): delta 7.34 (d, J=7.8 Hz, 1H), 7.04 (d, J=13.4 Hz, 1H), 5.25 (brs, 2H), 3.90 (s, 3H).

Statistics shows that 4-Fluoro-2-methoxyaniline is playing an increasingly important role. we look forward to future research findings about 450-91-9.

Reference of 702-24-9, 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. 702-24-9, name is 4-Methoxy-N-methylbenzylamine, This compound has unique chemical properties. The synthetic route is as follows.

A mixture of ethyl 8-bromo-6-chloroimidazo [1 ,2-b]pyridazine-3 -carboxylate (WO2009/100375) (5 g, 16.42 mmol), 1-(4-methoxyphenyl)-N-methylmethanamine (3.23 g,21.34 mmol), and N,N-diisopropylethylamine (5.74 ml, 32.8 mmol) in 1,4-dioxane (30 ml) was heated at 90 °C for 5 h. The volatiles were removed under vacuum. The residue was diluted with ethyl acetate (200 mL), washed with water (2 x 50 mL) and brine (50 mL), and dried over anhydrous Mg504. The desired product, ethyl 6-chloro-8-((4-methoxybenzyl)(methyl)amino)imidazo[ 1 ,2-b]pyridazine-3 -carboxylate (6.10 g, 16.27 mmol, 99 percent yield), was isolated as a pale yellow solid by ISCO (330 g silica gel, solid loading, 20-40percent ethyl acetate/hexane).

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

Synthetic Route of 101-84-8,Some common heterocyclic compound, 101-84-8, name is Diphenyl oxide, molecular formula is C12H10O, 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 12 (comparative)Decabromodiphenyl ether – Bromination of Deca completely dissolved in bromine.; The solubility of Deca in bromine was determined as 2.64 g Deca in 100 g bromine at 200C.To a 1 liter round bottomed flask equipped with a mechanical stirrer, a dropping funnel, a thermocouple and a reflux condenser was added 22 g of non milled Deca (content 97.1 %) and 1642 g bromine to produce a 1.32 % solution. AlBr3, 14.1 g, was added and the mixture was heated at reflux for 5 hours. After cooling to room temperature, water, 250 ml, was carefully added. The bromine was distilled and an additional 520 g of water was added. The solid was filtered and dried and consisted of 99.6 % Deca.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Diphenyl oxide, its application will become more common.

Synthetic Route of 150-78-7, 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 150-78-7 as follows.

General procedure: To a mixture of DITB (2, 517.7 mg, 1.10 mmol), oxone (681.0 mg, 1.11 mmol) in acetonitrile (4.5 mL) and HFIP (1.5 mL) was added 2-methoxynaphthalene (6c, 476.5 mg, 3.01 mmol), and the mixture was stirred for 24 h at 50 C. The reaction mixture was then diluted with ether and quenched with aqueous NaHCO3, and extracted with ether (15 mL x 3). The combined organic layers were washed with water (15 mL x 1), dried over Na2SO4, filtrated, and concentrated in vacuo. The residue was purified by silica gel column chromatography (eluent: hexane / chloroform = 5 / 1) to afford 1-bromo-2-methoxynaphthalene (7c, 578.5 mg, 81%) [S8].

According to the analysis of related databases, 150-78-7, the application of this compound in the production field has become more and more popular.

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. 4316-51-2, name is 4-Methoxytriphenylamine, A new synthetic method of this compound is introduced below., HPLC of Formula: C19H17NO

Example 14 Synthesis of 4-methoxy-4′,4″-diformyltriphenylamine: 5 g (18.16 mmol) of 4-methoxyltriphenylamine, 5.66 g (77.5 mmol) of N,N-dimethylformamide, 11.5 g (75.0 mmol) of phosphorus oxychloride, 2.5 g (18.3 nmmol) of zinc chloride, and 100 ml of toluene were subjected to reaction, post-treatment and isolation in the same manner as in Example 12. The results are set forth in Table 13. The reaction product exhibited the following physical properties:

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.

767-91-9, name is 2′-Methoxyphenyl acetylene, 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. Recommanded Product: 2′-Methoxyphenyl acetylene

General procedure: General produce: o-iodophenol (0.5 mmol), alkyne (1.0 mmol) andbase (1.0 mmol) were added into a 10 mL dry Schlenk tube under Ar,then anhydrous DMF (5 mL) was injected into the mixture using syringe.Then the solution stirred at preheated oil bath (160 C). The reactionwas monitored by TLC and GC.The mixture was cooled down toroom temperature after full conversion, then diluted with dichloromethaneand washed with water three times. The organic layerwas separated and washed with brine followed by drying with anhydrousNa2SO4. The filtrate was concentrated in vacuo to afford thecrude product, which was purified by flash column chromatography onsilica gel (petroleum ether).

The synthetic route of 767-91-9 has been constantly updated, and we look forward to future research findings.