Category: ethers-buliding-blocks

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. 701-07-5, name is 2-(2′-Bromophenoxy)propane, A new synthetic method of this compound is introduced below., Product Details of 701-07-5

An Et2O solution (10 mL) of I2 (1.21 g, 4.78 mmol) was added to a solid of 1 (0.72 g,0.79 mmol) to prepare the solution of diiodophenylarsine (2). Without isolation, thesolution of 2 was employed the subsequent reaction. To an Et2O solution (10 mL) of1-bromo-2-isopropoxybenzene (1.6 mL, 9.97 mmol) was added a hexane solution ofn-butyllithium (1.6 M, 6.0 mL, 9.6 mmol) at 0 C under N2 atmosphere, and the reactionmixture was stirred at the ambient temperature for 1 h. To the reaction mixture was thesolution of 2 was added at 0 C. The reaction temperature was raised to the ambienttemperature, and the reaction mixture was stirred for 5 h. The reaction was quenchedby distilled water (20 mL), and the products were extracted with EtOAc. The combinedorganic layers were dried over MgSO4, and volatiles were removed in vacuo. The residuewas subjected to recrystallization from EtOH, and washed with MeOH to obtaincolorless solids of 3c (1.52 g, 3.61 mmol, 72%). 1H NMR (CDCl3, 400 MHz) delta 7.34-7.24 (m,7H), 6.86 (t, J = 8.4 Hz, 2H), 6.83-6.77 (m, 4H), 4.50 (sep, J = 6.0 Hz, 2H), 1.18 (d, J = 6.0Hz, 6H), 1.08 (d, J = 6.4 Hz, 6H) ppm; 13C NMR (CDCl3, 100 MHz) delta 159.6, 139.9, 134.4,129.5, 129.4, 128.2, 127.9, 120.7, 112.1, 70.2, 21.9, 21.7 ppm. HR FAB-MS (m/z):calculated for C24H27O2As [M]+; 422.1227, observed; 422.1211.

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; Imoto, Hiroaki; Yamazawa, Chieko; Tanaka, Susumu; Kato, Takuji; Naka, Kensuke; Chemistry Letters; vol. 46; 6; (2017); p. 821 – 823;,
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Adding a certain compound to certain chemical reactions, such as: 7252-83-7, name is 2-Bromo-1,1-dimethoxyethane, 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 7252-83-7, Quality Control of 2-Bromo-1,1-dimethoxyethane

To a solution of 4-(diethylamino)benzothioamide (2.29 g, 11 mmol) in EtOH (60 mL) were added 2-bromo-1,1-dimethoxyethane (1.86 g, 11 mmol) and p-toluenesulfonic acid (1.89 g, 11 mmol). The reaction mixture was heated at 95 C. overnight, then cooled to rt and concentrated in vacuo. The residue was purified by a silica gel column chromatography (PE/EtOAc/Et3N (V/V/V)=2:1:0.05) to give the title compound as a white solid (1.40 g, 55%).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2-Bromo-1,1-dimethoxyethane, and friends who are interested can also refer to it.

Reference:
Patent; SUNSHINE LAKE PHARMA CO., LTD.; Zhang, Yingjun; Zhang, Jiancun; Wang, Xiaojun; Lin, Runfeng; Cao, Shengtian; Wang, Zhaohe; Li, Jing; US2015/87639; (2015); 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 398-62-9 as follows. HPLC of Formula: C8H9FO2

EXAMPLE 118 4-Chloro-1-[3,4-dimethoxy-6-fluorophenyl]-1-hexanone A solution of 0.1056 g (0.64 mmol) of 4-fluoroveratrole in 1 mL of methylene chloride was added to a mixture of 0.2289 g (1.7 mmol) of aluminum chloride and 0.09 mL (0.8 mmol) of 4-chlorobutyryl chloride in 2 mL of methylene chloride at 25. The reaction mixture was stirred at 25 for 22 hours. Water was added and the organic layer was separated and washed with sodium bicarbonate solution. The dried extract was concentrated under reduced pressure to an oil which was chromatographed on 10 g of silica gel using 25% ethyl acetatehexane to give 0.041 g, mp 81-82, of 4-chloro-[3,4-dimethoxy-6-fluorophenyl]-1-hexanone. The nmr spectrum was consistent with the structure and the mass spectrum gave the molecular ion at m/z 260 (C12 H14 ClFO3)

According to the analysis of related databases, 398-62-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Hoffmann-La Roche Inc.; US5025036; (1991); A;,
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Application of 175278-17-8, 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. 175278-17-8 name is 2-Bromo-4-(trifluoromethoxy)aniline, 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 anhydrous copper [(II)] chloride (6.3g, 47mmol) in acetonitrile (lOOmL) was added tert-butyl nitrite (6.85mL, [58MMOL),] followed dropwise by a solution of [2-BROMO-4- (TRIFLUOROMETHOXY)] aniline (lOg, 39mmol) in acetonitrile [(15ML).] The solution was stirred at ambient temperature for 1 hour then poured into hydrochloric acid (250mL, 2M). The suspension formed was extracted with diethyl ether [(2X250ML)] and the extracts were dried [(MGS04).] Concentration yielded the title compound as an oil (7.82g, [28MMOL).] [ON] (360 MHz, [CDCL3)] : 7.51 [(1H,] d, J 3.2Hz), 7.48 [(1H,] d, J 8.8Hz), 7.15 [(1H,] dd, J 3.2 and 8.8Hz).

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

Reference:
Patent; MERCK SHARP & DOHME LIMITED; WO2004/31190; (2004); 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 651734-54-2 as follows. Safety of 2,6-Difluoro-3,5-dimethoxyaniline

To a stirred slurry of 2,6-difluoro-3,5-dimethoxyaniline (500 mg, 2.64 mmol) in 6.0 M hydrogen chloride in water (4 mL, 24 mmol) was added a solution of sodium nitrite (191 mg, 2.78 mmol) in water (1 mL) dropwise over 15 min at 0 C. After stirring the resulting mixture at 0 C. for another 15 min, a solution of potassium iodide (1.8 g, 10. mmol) in water (2 mL) was slowly added to the resulting orange-red slurry at 0 C. with vigorus stirring. After completion of the addition, the reaction mixture was allowed to warm up to r.t. for 1 hour. The solid was collected by filtration, washed with water and dried under vacuum. 570 mg solid was collected and used directly in the next step.

According to the analysis of related databases, 651734-54-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Incyte Corporation; Li, Zhenwu; Wu, Liangxing; Yao, Wenqing; (48 pag.)US2017/320875; (2017); 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. 41365-75-7, name is 1-Amino-3,3-diethoxypropane, A new synthetic method of this compound is introduced below., Product Details of 41365-75-7

3,3-diethoxypropan-1-amine (6 g, 40.76 mmol, 1.00 equiv) was dissolved in1,4-dioxane (30 mL) in the presence of TEA (4.45 g, 43.98 mmol, 1.08 equiv), then cooled to 0C. (Boc)20 (9.6 g, 43.99 mmol, 1.08 equiv) diluted in 20 mL of 1,4- dioxane was added drop-wise. The solution was agitated 2 hours at 0C then overnight at ambient temperature before being neutralised with 10 mL of water. The pH was adjusted to 5 with HC1 (1 %). The solution was extracted 3 times with 50 mL of EtOAc.The organic phases were combined, dried over sodium sulfate, filtered and concentrated to yield 8.21 g (81 %) of compound 1ZD in the form of a pale yellow oil.

The synthetic route of 41365-75-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; PIERRE FABRE MEDICAMENT; PEREZ, Michel; RILATT, Ian; LAMOTHE, Marie; WO2014/174060; (2014); A1;,
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Adding a certain compound to certain chemical reactions, such as: 366-99-4, name is 3-Fluoro-4-methoxyaniline, 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 366-99-4, COA of Formula: C7H8FNO

General procedure: The procedure was performed adopting literature.46 To a solutionof ArNH2 (3, 5 mmol, dissolved in 10 mL acetic acid), wasadded aquatic solution of NaOCN (7.5 mmol, 7.5 mL). The mixturewas allowed to be stirred at room temperature for 1 h and thenconcentrated under reduced pressure. Afterwards, saturatedK2CO3 solution was added to adjust the pH to 7?8. A large scaleof precipitate was therefore formed, which was then filtered,washed with water for several times and then recrystallized fromMeOH – DCM

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:
Article; Zhang, Mao; Liang, Yu-Ru; Li, Huan; Liu, Ming-Ming; Wang, Yang; Bioorganic and Medicinal Chemistry; vol. 25; 24; (2017); p. 6623 – 6634;,
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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. 4003-89-8, name is 7-Methoxy-1,2,3,4-tetrahydronaphthalen-2-amine, A new synthetic method of this compound is introduced below., SDS of cas: 4003-89-8

(a) A solution of 1-[1-(p-toluenesulfonyl)indol-4-yloxy]-2,3-epoxypropane (3.9 g) and 2-amino-7-methoxytetralin (2.2 g) in isopropanol (40 ml) is refluxed for 3 hours. The reaction mixture is then evaporated to dryness, the residue is dissolved in ethyl acetate and the obtained solution is washed with water, dried over sodium sulfate and evaporated to dryness. The residue is taken up in ethyl acetate/isopropanol and the obtained solution is made acidic by the addition of HCl/isopropanol. The precipitate which forms is recovered by filtration, and suspended in hot ethanol. The suspension is then cooled and filtered and the solid recovered by filtration is dried yielding 3.1 g of N-(7-methoxy-1,2,3,4-tetrahydronaphth-2-yl)-2-hydroxy-3-[1-(p-toluenesulfonyl)indol-4-yloxy]propanamine hydrochloride; m.p. 228-231 C.

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; Elf Sanofi; US5254595; (1993); A;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

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 645-36-3 as follows. Recommanded Product: 2,2-Diethoxyethanamine

[00231] To a solution of cyanogen bromide (25 g, 236.03 mmol) in hexane (80 mL) was added a solution of the amino-acetaldehyde diethyl acetal (34.3 mL, 236.03 mmol) in diethyl ether (80 mL) at room temperature. The resulting mixture was stuffed overnight. A white solid was formed and was removed by filtration and washed with diethyl ether. The filtrate was concentrated and purified by flash chromatography on silica gel (eluted with 0/100 to 5/95 methanol/dichloromethane) to afford N- (2,2-diethyloxyethyl)carbodiimide (27 g, 72% yield) as a bright yellow oil. Rt (retention time) = 1.82 mm; MS m/z: 159.20 [M+1].

According to the analysis of related databases, 645-36-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; DANA-FARBER CANCER INSTITUTE, INC.; CHOI, Hwan, Geun; LIANG, Yanke; GRAY, Nathanael; (135 pag.)WO2016/14542; (2016); A1;,
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Reference of 115144-40-6, 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 115144-40-6 as follows.

1, 2-Difluoro-4-methoxy-benzene (100mg, 0. 69MMOL) and sodium methan- ethiolate (148mg, 2. 08MMOL) were dissolved in N, N-dimethylformamide (2mL) and the reaction mixture stirred at 60C for 18 hours. Additional sodium METHANETHIOLATE (99mg, 139MMOL) was added and the reaction mixture was heated to 100C for 18 hours. The reaction mixture was diluted with water and extracted with ether (x 2). The ether extracts were washed with water (x 2), dried (MGS04) and then concentrated under reduced pressure. The residue was taken up in a pentane: ether 1: 1 solution (2mL) and filtered through a plug of silica in a pipette, and then washed through with a pentane: ether 1: 1 solution (5mL). The solution was concentrated under reduced pressure to yield the title product as a colourless oil, 135mg. H NMR (CDCI3, 300MHZ) 8 : 2.45 (s, 3H), 3.80 (s, 3H), 6.65 (dd, 1H), 6.80 (DD, 1 H), 6.95 (dd, 1 H).

According to the analysis of related databases, 115144-40-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; PFIZER LIMITED; PFIZER INC.; WO2005/9964; (2005); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem