Tag: M.W=100-200

Adding a certain compound to certain chemical reactions, such as: 710-18-9, name is 1-Methoxy-4-(trifluoromethoxy)benzene, 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 710-18-9, Recommanded Product: 1-Methoxy-4-(trifluoromethoxy)benzene

Preparation 34 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 Na2SO4, 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.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Patent; Aventis Pharmaceuticals Inc.; US6194406; (2001); B1;,
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366-99-4, name is 3-Fluoro-4-methoxyaniline, 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. Product Details of 366-99-4

Reference Example 13; N- (5-Fluoro-4-methoxy-2-nitrophenyl) acetamide; Acetic anhydride (5 ml) was added to 3-fluoro-4- methoxyaniline (5.0 g), and the mixture was stirred for 30 minutes. The reaction mixture was cooled to room temperature, and nitric acid (2.3 ml) was added dropwise thereto. The mixture was stirred for 30 minutes, and water was added thereto. The resulting precipitate was collected and washed with water to obtain the title compound as crystals (5.7 g, 71percent). H-NMR (300 MHz, CDC13) 5 (ppm): 2.29 (3H, s), 3.94 (3H, s), 7.80 (1H, d, J=8. 4Hz), 8.66 (1H, d, J=10.5Hz), 10.39 (1H, brs).

The synthetic route of 366-99-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; TAKEDA PHARMACEUTICAL COMPANY LIMITED; WO2005/82879; (2005); A1;,
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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. 13101-88-7, name is 6-Methoxynaphthalen-2-amine, A new synthetic method of this compound is introduced below., Quality Control of 6-Methoxynaphthalen-2-amine

Weigh compound 6-methoxy-2-naphthyl-amine (7g, 0.04044mol), triethylamine (6g, 0.06067mol) in 100mL reaction flask, a solution of methylene chloride was added to the reaction flask of 15mL at 0 the reaction conditions under 15min; dropwise added methanesulfonyl chloride (7g, 0.06067mol), under reaction conditions 0 30min, TLC plate monitor, the reaction was complete, adding an appropriate amount of aqueous sodium hydroxide solution, extracted with ethyl acetate and saturated brine dried over anhydrous sodium sulfate, and spin dry, column chromatography (PE: EA = 2: 1), give a purple solid 5.6g, yield 55.2%.

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.

Reference:
Patent; East China University of Science and Technology; Li, Hongling; Jiang, Hualiang; Xu, Yufang; Li, Jia; Zhao, Zhenjang; Li, Jingya; Xu, Hongling; Li, Shiliang; (64 pag.)CN105566276; (2016); A;,
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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. 10541-78-3, name is 2-Methoxy-N-methylaniline, A new synthetic method of this compound is introduced below., HPLC of Formula: C8H11NO

General procedure: A mixture of secondary amine 1 (200 mg, 1 equiv), polyformaldehyde 2 (1.5 equiv) and the activated alkene 3 (1.1 equiv) was dissolved in acetonitrile (2 mL). The solution was stirred at room temperature for 3 days until the starting secondary amine 1 was no longer detected by TLC (revealed with an ethanolic solution of vanillin-sulfuric acid or iodine). After the excess of solvent was removed under reduced pressure, the oily material obtained was purified by column chromatography on silica gel (70-230 mesh), using CHCl3:MeOH mixtures of (30:1, 20:1 or 15:1) as eluent.

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.

Reference:
Article; Abonia, Rodrigo; Castillo, Juan C.; Garay, Alexander; Insuasty, Braulio; Quiroga, Jairo; Nogueras, Manuel; Cobo, Justo; D’Vries, Richard; Tetrahedron Letters; vol. 58; 15; (2017); p. 1490 – 1494;,
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Application of 592-55-2,Some common heterocyclic compound, 592-55-2, name is 1-Bromo-2-ethoxyethane, molecular formula is C4H9BrO, 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.

Under ice-cooling, sodium hydride (60% in oil, 1.44 g, 36.0 mmol) was added to a solution of 3-bromo-2-methyl-1H-indole (6.30 g, 30.0 mmol) in N,N-dimethylformamide (30 mL) by small portions, and the mixture was stirred under a nitrogen atmosphere at the same temperature for 1 hr. To the reaction mixture were added 2-bromoethyl ethyl ether (5.07 mL, 45.0 mmol) and sodium iodide (0.747 g, 4.50 mmol), and the mixture was stirred at 70C for 6 hr. The reaction mixture was concentrated under reduced pressure, water was added and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane-25% ethyl acetate/hexane) to give the title compound (6.30 g, yield 74%) as dark-purple oil. MS m/z 282 (MH+).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-Bromo-2-ethoxyethane, its application will become more common.

Reference:
Patent; Takeda Pharmaceutical Company Limited; EP1726580; (2006); A1;,
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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 634-36-6 as follows. Safety of 1,2,3-Trimethoxybenzene

1-Bromo-2,3,4-trimethoxy-benzene (9) Pyrogallol trimethyl ether (5.1 g) was suspended in CCl4 (60 mL) and N-bromosuccinimide (6.5 g, 1.2 eq.) was added. The reaction mixture was heated at reflux for 20 hours. The succinimide was collected and the filtrate concentrated in vacuo to a brown oil. The oil was separated by gravity column chromatography (hexane-ethyl acetate, 19: 1) and yielded the title compound as a yellow oil (5.9 g, 78%): EIMS m/z 234 ((M+ -CH3, 81Br), 232 (M+ -CH3, 79Br), 107, 95, 69, 58, 44; 1H NMR (CDCl3, 300 MHZ) delta 7.21 (1H, d, J=9.0 Hz, H6), 6.58 (1H, d, J=9.0 Hz, H5), 3.91 (3H, s, OCH3), 3.89 (3H, s, OCH3), 3.85 (3H, s, OCH3).

According to the analysis of related databases, 634-36-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Pettit, George R.; Grealish, Matthew P; US2003/220304; (2003); A1;,
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Adding a certain compound to certain chemical reactions, such as: 3616-56-6, name is 2,2-Diethoxy-N,N-dimethylethanamine, 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 3616-56-6, category: ethers-buliding-blocks

(3) 1H,1’H-2,3′-biindole (16.4 g, 70.6 mmol) and 2,2-diethoxy-N,N-dimethylethanamine (14.18 ml, 78 mmol) in glacial acetic acid (160 mL) were refluxed at 130 °C overnight under nitrogen. The reaction solution was cooled to room temperature and filtered. The filtrate was washed with small amount of acetic acid and excess of water. The filtrate was dried in the oven at 65°C overnight affording 10.79 g (60percent) of the 5,12-dihydroindolo[3,2-a]carbazole as gray 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, 2,2-Diethoxy-N,N-dimethylethanamine, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Universal Display Corporation; Joseph, Scott; Boudreault, Pierre-Luc T.; Dyatkin, Alexey Borisovich; Li, David Zenan; Xia, Chuanjun; Yamamoto, Hitoshi; EP2910555; (2015); A1;,
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Electric Literature of 111-95-5,Some common heterocyclic compound, 111-95-5, name is Bis(2-methoxyethyl)amine, molecular formula is C6H15NO2, 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 an ethanolic solution (30 ml) of p-chlorophenol (30 mmol, 3.86 g), bis(2-methoxyethyl)amine (90 mmol, 11.99 g) was added dropwise with constant stirring. After 30 min, 37% (w/v) formalin solution (90 mmol, 7.5 ml) was added to it. The resulting mixture was stirred for 1 h at room temperature and then refluxed for 24 h. Then the same procedure-was followed as for HL1. The liquid ligand was further purified by flash column chromatography (silica gel, hexane:ethylacetate:triethylamine=100:5:1) to afford the desired beta-aminophenol.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Bis(2-methoxyethyl)amine, its application will become more common.

Reference:
Article; Sanyal, Ria; Chakraborty, Prateeti; Zangrando, Ennio; Das, Debasis; Polyhedron; vol. 97; (2015); p. 55 – 65;,
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Related Products of 39538-68-6, 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. 39538-68-6 name is 2-Methoxy-4-methylaniline, 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.

A solution of sodium nitrite (7 g, 101.4 mmol) in water (25 ml) was added dropwise to a cooled (0-5C) solution of Intermediate 1A (13.7 g, 100 mmol) in concentrated hydrochloric acid (30 ml) and water (85 ml). After stirring at 0C for 10 min, sodium acetate (15 g, 182.8 mmol) was added. The resulting mixture was added dropwise to a hot solution (70-80C) of potassium O-ethyl dithio- carbonate (30 g, 187.1 mmol) in water (140 ml), stirred between 70C and 80C for 1 h and then cooled to rt. The mixture was extracted twice with ethyl acetate, and the combined organic extracts were dried over sodium sulfate and evaporated. The residue was taken up in a 1.3 M solution of potassium hydroxide in ethanol (300 ml). Glucose (8 g) was added, and the resulting mixture was refluxed for 3 h. Then, the ethanol solvent was evaporated, and the residue was diluted with water and acidified with 6 N aqueous sulfuric acid. Zinc powder (15 g) was added carefully, and the resulting mixture was heated to 50C for 30 min. The mixture was then cooled to rt, diluted with dichloromethane and filtered. The filtrate was extracted twice with dichloromethane, and the combined organic extracts were dried over sodium sulfate and evaporated affording 14.3 g of the crude product which was used in the next step without further purification.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2-Methoxy-4-methylaniline, and friends who are interested can also refer to it.

Reference:
Patent; BAYER INTELLECTUAL PROPERTY GMBH; BAYER PHARMA AKTIENGESELLSCHAFT; COLLIN, Marie-Pierre; BROHM, Dirk; HEROULT, Melanie; LOBELL, Mario; HUeBSCH, Walter; LUSTIG, Klemens; GRUeNEWALD, Sylvia; BOeMER, Ulf; VOeHRINGER, Verena; LINDNER, Niels; WO2013/87647; (2013); A1;,
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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. 14869-41-1, name is 2-(2-Chloroethoxy)acetic acid, This compound has unique chemical properties. The synthetic route is as follows., Safety of 2-(2-Chloroethoxy)acetic acid

I.1.4. 2-(1-Piperazinyl)ethoxyacetic Acid 8.6 g (0.1 mol) of piperazine, 17.7 g (0.1 mol) of piperazine dihydrochloride and 50 ml of water are introduced into a 100 ml three-necked round-bottomed flask fitted with a water-cooled condenser and a mechanical stirrer. The mixture is brought to a temperature of 70° C. 15.2 g of (2-chloroethoxy) acetic acid are then added dropwise over 15 minutes. The mixture is brought to a temperature of 80° C. with stirring and is maintained at this temperature for 27 hours. The mixture is allowed to cool to room temperature and the water is evaporated off under reduced pressure on a rotary evaporator. The evaporation residue is taken up in 50 ml of ethanol and maintained at 50° C. with stirring for 45 minutes. It is then placed in an ice bath and is stirred for 1 hour. The precipitate (piperazine dihydrochloride) formed is then filtered off and the solvents are evaporated off under reduced pressure on a rotary evaporator at 50° C. 22.4 g of a yellow oil are obtained. 10 g of this mixture are purified on 130 g of Amberlyte IRA-400 resin. Elution is carried out first with 600 ml of water and then with aqueous 0.5 M ammonium acetate solution. The fractions containing the 2-(1-piperazinyl)ethoxyacetic acid or its salt are combined and the water is removed therefrom under reduced pressure at 60° C. on a rotary evaporator. 18.2 g of a mixture containing white crystals and an oil are recovered. This mixture is taken up in 75 ml of isopropanol and the insoluble crystals are filtered off. The filtrate is acidified with 20 ml of a 9N solution of hydrochloric acid in ethanol. The precipitate formed is filtered off quickly, washed with isopropanol and dried on a rotary evaporator under reduced pressure at 50° C. 7.1 g of a white solid are obtained, which solid is purified by subliming the ammonium chloride salts (4 hours at 135° C. under 0.1 mbar and then 8 hours at 150° C. under 0.1 mbar). 1.4 g of 2-(1-piperazinyl)ethoxyacetic acid dihydrochloride are thus obtained. Yield: 12percent NMR: delta: 2.36 (2H, t, 4.8 Hz); 3.45 (4H, m); 3.53 (4H, m); 3.88 (2H, t, 4.8 Hz); 4.09 (2H, s); 10 (1H, bs). Mass spectrum: 189 (MH+)

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 14869-41-1.

Reference:
Patent; UCB, S.A.; US6140501; (2000); A;,
Ether – Wikipedia,
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