Author: tianli

Adding a certain compound to certain chemical reactions, such as: 144284-25-3, 2,4,5-Trifluorobenzyl alcohol, 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, 144284-25-3, blongs to alcohols-buliding-blocks compound. Computed Properties of C7H5F3O

General procedure: Triphenylphosphonium salts 49 and 50 were obtained by treating alcohols 47 and 48 (4.5 mmol) in MeCN/THF (1:1, 10 mL) with Ph3P.HBr (3.12 g, 9 mmol). The resulting reaction mixture was heated at 80 C to complete the reaction (as indicated by TLC). The solvents were evaporated and the oily residues were triturated with Et2O. After overnight refrigeration and filtration of the precipitates, the corresponding salts were obtained and used without further purification.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,144284-25-3, its application will become more common.

Reference:
Article; Magoulas, George E.; Bariamis, Stavros E.; Athanassopoulos, Constantinos M.; Haskopoulos, Anastasios; Dedes, Petros G.; Krokidis, Marios G.; Karamanos, Nikos K.; Kletsas, Dimitris; Papaioannou, Dionissios; Maroulis, George; European Journal of Medicinal Chemistry; vol. 46; 2; (2011); p. 721 – 737;,
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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. 431-23-2, name is 3,3,3-Trifluoro-2-methylpropan-1-ol. A new synthetic method of this compound is introduced below., COA of Formula: C4H7F3O

To a solution of 3,3,3-trifluoro-2-methylpropan-1-ol (800 mg, 6.25 mmol) in DCM (20 mL) was added triethylamine (950 mg, 9.39 mmol).The reaction mixture was cooled to -20 C,Then trifluoromethanesulfonic anhydride (2.20 g, 7.70 mmol) was added to the above system.The reaction was stirred at 0 & lt; 0 & gt; C overnight.The reaction mixture was diluted with DCM (50 mL)And then washed with 1 M aqueous hydrochloric acid (50 mL x 2)The separated organic phases were dried over anhydrous sodium sulfate and concentrated under reduced pressure to give the title compound as a yellow oil(1.1 g, 68% yield).

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, 431-23-2, 3,3,3-Trifluoro-2-methylpropan-1-ol.

Reference:
Patent; Sunshine Lake Pharma Co., Ltd.; Xi, Ning; Dai, Weilong; Li, Minxiong; Chen, Wuhong; Zhang, Tao; Hu, Haiyang; Li, Xiaobo; Liu, Jun; Wang, Tingjin; (146 pag.)CN106478651; (2017); A;,
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Application of 17366-48-2 , The common heterocyclic compound, 17366-48-2, name is exo-8-Azabicyclo[3.2.1]octan-3-ol hydrochloride, molecular formula is C7H14ClNO, 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.

8-Aza-bicyclo [3.2. 1] octanol hydrochloride (5.1 g, 31.45 mmol)) and sodium carbonate (13.3 g, 125.8 mmol) are suspended in 150 mi of ethanol at room temperature. 2-Bromo- ethanol (4.4 ml, 62.9 mmol) is added dropwise within 20 minutes and the reaction mixture is refluxed for 15 hours. After cooling to room temperature the reaction mixture is evaporated under reduced pressure. The mixture is stirred with 200 ml of DCM and filtered. The clear filtrate is dried over anhydrous sodium sulfate, filtered, evaporated under reduced pressure und dried at high vacuum. Yield : 5.4 g (100%) of a colorless oil. MS (ESI) : 172 [M+H] +, 1 H-NMR (DMSO-d6) : 5 (ppm) 4.25 (d, 2H), 3.78 (t, 1H), 3.42 (t, 2H), 3.06 (m, 2H), 2.36 (t, 2H), 2.03 (m, 2H), 1.85 (m, 2H), 1.75 (m, 2H), 1. 55 (d, 2H).

The synthetic route of 17366-48-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; NOVARTIS AG; NOVARTIS PHARMA GmbH; WO2005/77932; (2005); A2;,
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Related Products of 18684-63-4, With the rapid development and complex challenges of chemical substances, the synthesis of new drugs is usually one of the most effective ways to increase yield.18684-63-4, name is Bicyclo[2.2.2]octan-2-ol, molecular formula is C8H14O, molecular weight is 126.2, as common compound, the synthetic route is as follows.

Preparation of bicyclo[2.2.2]octan-2-one (7) A mixture of bicyclo[2.2.2]octan-2-ol 6 (0.710 g, 5.72 mmol) and 1-hydroxy-1,2-benziodoxol-3H-one-1-oxide (2.40 g, 8.59 mmol) in dichloroethane (20 mL) was refluxed for 1 h, filtered through a pad of celite, washed with dichloromethane and concentrated to provide 7 (0.62 g, 87%) as a white solid. 1H NMR (400 MHz, CDCl3): delta 1.62 (2H, m), 1.70 (2H, m), 1.82 (4H, m), 2.15 (1H, m), 2.25 (3H, m)

The chemical industry reduces the impact on the environment during synthesis 18684-63-4, I believe this compound will play a more active role in future production and life.

Reference:
Patent; Naeja Pharmaceutical Inc.; US2011/288063; (2011); A1;,
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Synthetic Route of 13588-28-8, With the rapid development and complex challenges of chemical substances, the synthesis of new drugs is usually one of the most effective ways to increase yield.13588-28-8, name is 2-(2-Methoxypropoxy)propan-1-ol, molecular formula is C7H16O3, molecular weight is 148.2001, as common compound, the synthetic route is as follows.

In a 500 mL flask, flake-like sodium hydroxide (manufactured by Tosoh Corporation) (hereinafter also referred to as”NaOH tablets”) 51.5 g (relative to the following DPMI moles,Equivalent to 1. 4 moles)And 1-bromopropane (manufactured by Wako Pure Chemical Industries, Ltd.) (hereinafter also referred to as “PrBr”) 144.2 g(Relative to the following DPMI moles,Equivalent to 1. 3 moles)Start stirring.After raising the liquid temperature to 35 C,While keeping the temperature inside the system at 35 C,(Hereinafter referred to as “DPM”) was added dropwise over 6 hours to a solution of 133.7 g of dipropylene glycol monomethyl ether (isomer mixture) (manufactured by Wako Pure Chemical Industries, Ltd.).Thereafter,The overnight stirring was carried out while maintaining the temperature of 35 C.In addition,The amount of propylene gas as a low boiling compound produced in the above reaction was measured using a gas flow meter.The reaction solution was added with water 118. After 5 g, extraction /The resulting organic phase 194. 6 g was analyzed by gas chromatography,As a result, it was found that dipropylene glycol methyl n-propyl ether (isomer mixture) (hereinafter also referred to as “DPMNP”) 136.3 g (DPM basis yield: 79.4%, PrBr basis yield: 61 . 1% ).

Statistics shows that 13588-28-8 is playing an increasingly important role. we look forward to future research findings about 2-(2-Methoxypropoxy)propan-1-ol.

Reference:
Patent; Daicel Corporation; Mori, Atsushi; (9 pag.)CN105503545; (2016); A;,
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Adding a certain compound to certain chemical reactions, such as: 21285-46-1, (E)-2,3-Dibromobut-2-ene-1,4-diol, 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, Recommanded Product: (E)-2,3-Dibromobut-2-ene-1,4-diol, blongs to alcohols-buliding-blocks compound. Recommanded Product: (E)-2,3-Dibromobut-2-ene-1,4-diol

10128] Propargyl bromide (80% solution in toluene, 1.25 mE, 11.6 mmol, 1 equiv) was added to a stirred solution of (E)-2,3-dibromobut-2-ene-1,4-diol (51, 8.56 g, 34.8 mmol, 3.00 equiv) and potassium hydroxide (1.30 g, 23.2 mmol,2.00 equiv) in 50% N,N-dimethylformamide-water (30 mE) at 24 C. The resulting mixture was stirred for 12 hat 24 C. The product mixture was purified by flash-column chromatography (eluting with 25% ethyl acetate-hexanes, grading to 100% ethyl acetate, one step) to afford (E)-2,3-dibromo-4- (prop-2-yn-1-yloxy)but-2-en-1-ol (S2) as a white solid (2.69 g, 82%). R1=0.26 (20% ethyl acetate-hexanes; CAM). ?H NMR (400 MHz, CDC13): oe 4.49 (s, 4H, H,/H2), 4.14 (d, 2H, J=2.4 Hz, H3), 3.28 (t, 1H, J=6.8 Hz, OH), 2.49 (t, 1H, J=2.4 Hz, H4). ?3C NMR (600 MHz, CDC13): oe 125.3 (C), 118.6 (C), 78.8 (C), 75.5 (CH), 72.8 (CH2), 66.8 (CH2), 57.2 (CH2). IR (NaC1), cm?: 3295 (br), 1092 (m), 642 (m). HRMS-ESI (m/z): [M+H] calculated for C7H8798?Br2O2, 283.8871. found, 283.8878.

The synthetic route of 21285-46-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; The Regents of the University of California; Bertozzi, Carolyn R.; Woo, Christina; (50 pag.)US2016/187350; (2016); A1;,
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Reference of 125617-18-7, The major producers of chemicals have been the Europe, Japan and China. Due to the growing call for a cleaner, greener environment, people will have to find innovative ways to maintain their relevance. Here is a compound 125617-18-7, name is (E)-3-(4-(Trifluoromethyl)phenyl)prop-2-en-1-ol. This compound has unique chemical properties. The synthetic route is as follows.

(2E)-3-[4-(Trifluoromethyl)phenyl]-2-propen-1-ol (242 mg), methyl 3-(2-aminophenoxy)benzoate (243 mg), triphenyl phosphine (11 mg) and molecular sieves 4A (200 mg) were suspended in benzene (5 mL) under an argon atmosphere. Titanium (IV) isopropoxide (150 muL) and palladium acetate (6 mg) were added to the suspension and heated to reflux for 3 hours. The reaction mixture was cooled down to room temperature, 1N hydrochloric acid was added thereto and the mixture was extracted with ethyl acetate. 1N Sodium hydroxide was added to the aqueous layer to make alkaline and the mixture was extracted with ethyl acetate again. The organic layers were combined, successively washed with water and saturated saline solution, dried over anhydrous sodium sulfate and concentrated. The resulting residue was purified by a silica gel column chromatography (hexane : ethyl acetate = 20:1) to give methyl ester of the title compound (methyl 3-[2-({(2E)-3-[4-(trifluoromethyl)phenyl]-2-propenyl}amino)phenoxy]benzoate). The same operation as Example 4 was carried out using the methyl ester of the title compound instead of the compound produced in Example 3 to give the compound of the present invention (232 mg) having the following properties. TLC: Rf 0.35 (dichloromethane:methanol = 19:1); NMR (DMSO-d6) delta 3.95, 5.68, 6.41-6.55, 6.56-6.65, 6.75, 6.89, 6.99-7.09, 7.19-7.30, 7.38, 7.47, 7.55, 7.59-7.67, 13.06.

According to the analysis of related databases, 125617-18-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ONO PHARMACEUTICAL CO., LTD.; EP1661879; (2006); A1;,
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Application of 205877-13-0 ,Some common heterocyclic compound, 205877-13-0, molecular formula is C8H11NO2, 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.

General procedure: A solution of 4-toluene sulfonyl chloride (4.58 g, 1.2 equiv) or methanesulfonyl chloride (1.9 mL, 1.2 equiv) and pyridine (2 mL, 1.3 equiv) in 20 mL CH2Cl2 was added slowly to the solution of compound 11 (0.02 mol) in 40 mL CH2Cl2. The mixture was stirred overnight at room temperature. Then 30 mL diluted HCl solution was added to the reaction mixture, the organic layer was separated using separating funnel. Subequently, the aqueous phase was extracted with 15 mL CH2Cl2 three times, the combined organic layers were washed separately with saturated NaHCO3 (30 mL) and saturated NaCl (30 mL) three times. The organic layer was dried over Na2SO4, filtered and evaporated under reduced pressure. The residue was purified by column chromatography using petroleum ether/EtOAc = 1/1 to give the product 12.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,205877-13-0, its application will become more common.

Reference:
Article; Xu, Changrui; Wu, Zhengxing; Chen, Jianzhong; Xie, Fang; Zhang, Wanbin; Tetrahedron; vol. 73; 14; (2017); p. 1904 – 1910;,
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Reference of 81156-68-5, With the rapid development and complex challenges of chemical substances, the synthesis of new drugs is usually one of the most effective ways to increase yield.81156-68-5, name is 2,4-Dichlorophenethyl alcohol, molecular formula is C8H8Cl2O, molecular weight is 191.06, as common compound, the synthetic route is as follows.

(ii) 3-[2-(2,4-Dichlorophenyl)-Ethoxy]-4,5-Dimethoxy-Benzoic Acid 2 g (9.42 mmol) of 3-Hydroxy-4,5-dimethoxy-benzoic acid methyl ester was dissolved in 100 ml of anhydrous tetrahydrofuran. To this solution was added 1.98 g (10.37 mmol) of 2-(2,4-Dichlorophenyl)-ethanol, 9.415 g (equivalent to 28.27 mmol PPh3) of triphenylphosphine derivatized polystyrene and 4.924 g (28.27 mmol) of DEAD. The solution was shaken for 16 h at RT. The polymer was filtered off and washed with ethyl acetate. The solvent was removed under reduced pressure. The residue was taken-up in ethyl acetate and the solution was washed three times with water and twice with saturated aqueous sodium chloride. The organic phase was dried with magnesium sulphate, filtered and the solvent was removed under reduced pressure. The residue was dissolved in 20 ml of dioxan. 1 ml of water was added to the solution followed by 2N aqueous NaOH to give a pH of 13. The reaction solution was heated at 60 C. for 10 hours. The solution was cooled to 0 C., 5 ml water was added, followed by concentrated hydrochloric acid to give a pH of 1 to 2, whereupon the product precipitated from solution. The product was filtered off and dried under reduced pressure.

The chemical industry reduces the impact on the environment during synthesis 81156-68-5, I believe this compound will play a more active role in future production and life.

Reference:
Patent; Nazare, Marc; Will, David William; Peyman, Anuschirwan; Matter, Hans; Zoller, Gerhard; Gerlach, Uwe; US2002/198195; (2002); A1;,
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Reference of 1013031-65-6, 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 1013031-65-6 as follows.

To a solution of (2,6-dibromophenyl)methanol (5 g, 18.8 mmol) in dichloromethane (50 mL) was added te^butylchlorodimethylsilane (4.25 g, 28.2 mmol) and lH-imidazole (1.91 g, 28.2 mmol) at 0 C. The reaction was stirred at ambient temperature for 16 h. Upon completion, the mixture was washed with water (3 x 100 mL), the organic layer was dried over Na2S04. The organic layer was filtered and concentrated to dryness. Purification by column chromatography (PE) gave the product (7 g, yield: 95%).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,1013031-65-6, its application will become more common.

Reference:
Patent; SUNOVION PHARMACEUTICALS INC.; BOWEN, Carrie, A.; BURDI, Douglas, F.; HEFFERNAN, Michele, L., R.; HERMAN, Lee, W.; XIE, Linghong; (266 pag.)WO2019/28165; (2019); A1;,
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