Month: March 2021

Synthetic Route of 756520-66-8, 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. 756520-66-8, name is 1-(2,6-Dichloro-3-fluorophenyl)ethanol. A new synthetic method of this compound is introduced below.

A solution of 1- (2,6-dichloro-3-fluorophenyl) ethanol (5 g, 23.9 mmol) in hydrobromic acid (30 ml) When cooled to room temperature. Extracted with ethyl acetate. The combined organic phases were washed with water, dried over anhydrous sodium sulfate and concentrated to give the product (5.2 g, Yield: 80%).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,756520-66-8, 1-(2,6-Dichloro-3-fluorophenyl)ethanol, and friends who are interested can also refer to it.

Reference:
Patent; Tianjin Binjiang Pharmaceutical Inc.; Tian, Hongqi; Huang, Gongchao; (33 pag.)CN103497177; (2017); B;,
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Electric Literature of 599-67-7, 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. 599-67-7, name is 1,1-Diphenylethanol, molecular formula is C14H14O, The 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.

General procedure: Iodine (5.1 mg, 0.02 mmol) was added to phenol 1l (0.148 g, 1 mmol) or alcohol 3h (0.242 g, 1 mmol), followed by addition of HMDS (0.089 g, 0.55 mmol); the mixture was stirred at room temperature until the complete consumption of the starting material (TLC check). The crude reaction mixture was dissolved in 4 mL of hexane/TBME and stirred with the finely powdered Na2S2O3 until the disappearance of iodine. From this point on, two different scenarios are possible: a) The solids were filtered off and the solvent evaporated under the reduced pressure, yielding the crude product. In numerous cases, such products were practically pure; column chromatography and/or distillation improved their quality only slightly. b) A solution of a product in hexane/TBME mixture could be directly subjected to the column chromatography, without filtration of the solids. Caution: Although we experienced no problems when performing these reactions, care should taken due to the potential formation of NI3.

While traditionally a conservative industry, chemical producers will need to modernize their PR strategies to stay relevant.we look forward to future research findings about 599-67-7, 1,1-Diphenylethanol.

Reference:
Article; Jereb, Marjan; Tetrahedron; vol. 68; 20; (2012); p. 3861 – 3867;,
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Adding a certain compound to certain chemical reactions, such as: 1124-63-6, 3-Cyclohexylpropan-1-ol, 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, SDS of cas: 1124-63-6, blongs to alcohols-buliding-blocks compound. SDS of cas: 1124-63-6

2.2 M diethyl azodicarboxylate (1.01 ml) and triphenylphosphine (581 mg) were added to a THF (20 ml) solution containing the resulting compound (450 mg) and 3-cyclohexyl-1-propanol (315 mg), followed by heating at 50C for 22 hours. Water was added to the reaction solution, followed by extracttion with chloroform. The organic layer was washed with saturated brine and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (eluent: hexane:EtOAc = 2:1 (v/v)) to obtain methyl 5-[({4-[4[(3-cyclohexylpropoxy)phenoxy]piperidin-1-yl}carbonyl)oxy]nicotinate (242 mg).

The synthetic route of 1124-63-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Astellas Pharma Inc.; EP1849773; (2007); A1;,
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Related Products of 7735-42-4, 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.7735-42-4, name is 1,16-Hexadecanediol, molecular formula is C16H34O2, molecular weight is 258.44, as common compound, the synthetic route is as follows.

The acetone is then evaporated off with the rotary evaporator, the residue is taken up in ethyl ether and water and the product is extracted three times with ether. The ethereal phases are combined and are dried over magnesium sulphate. The white solid obtained is then recrystallized from methanol (M.p. 42-43 C.). Yield=95%. 1,16-diiodohexadecane is obtained from hexadecane-1,16-diol, by adding 5 g of this diol and 19 g of potassium iodide to a solution of 2.5 g of phosphoric anhydride and 5.2 mL of 85% phosphoric acid. The mixture is heated at 100 C. for 5 hours. A dense oil forms, and the mixture is poured into 50 mL of water. The organic phase is separated, and the aqueous phase extracted with ether. The organic phases are discoloured by stirring with 50 mL of a 10% solution of sodium thiosulphate. The ether is evaporated off. The oil obtained is crystallized from methanol (M.p.=52 C.). Yield: 82%.

The chemical industry reduces the impact on the environment during synthesis 7735-42-4, I believe this compound will play a more active role in future production and life.

Reference:
Patent; CNRS; US6972343; (2005); B1;,
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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 756520-66-8, name is 1-(2,6-Dichloro-3-fluorophenyl)ethanol. This compound has unique chemical properties. The synthetic route is as follows. Product Details of 756520-66-8

To a solution of 1-(2,6-dichloro-3-fluorophenyl)ethan-1-one 11 (20.00 g, 96.60 mmol) in 100 mL of MeOH was added portionwise NaBH4 (7.31 g, 193.21 mmol). The resulting mixture was stirred at room temperature for 2 h and then quenched with 20 mL of water. After the removal of MeOH under vacuum, the residue was extracted with EA and washed with brine. The organic layer was dried over anhydrous Na2SO4 and concentrated under vacuum to afford 1-(2,6-dichloro-3-fluorophenyl)ethan-1-ol, which was pure enough for use in the next step. 1H NMR (400 MHz, CDCl3) delta 7.26 (dd, J = 4.8, 8.8 Hz, 1H), 7.02 (dd, J = 8.0, 8.8 Hz, 1H), 5.57 (q, J = 6.8 Hz, 1H), 2.86 (br, 1H), 1.64 (d, J = 6.8 Hz, 3H). To a solution of 1-(2,6-dichloro-3-fluorophenyl)ethan-1-ol (19.00 g, 90.89 mmol) in 150 mL of CH2Cl2 was added Et3N (13.27 mL, 95.43 mmol) and catalytic amount of DMAP. The resulting solution was cooled in an ice bath and added dropwise MsCl (7.39 mL, 95.43 mmol). After complete addition of MsCl, the reaction mixture was maintained in the ice bath for 1 h and then 30 mL of water was added to the reaction mixture. The organic phase was washed with brine, dried over anhydrous Na2SO4 and concentrated under vacuum to afford 1-(2,6-dichloro-3-fluorophenyl)ethyl methanesulfonate (12), which was pure enough for use in the next step. Yield: 84%; 1H NMR (300 MHz, CDCl3) delta 7.33 (dd, J = 4.8, 9.0 Hz, 1H), 7.12 (dd, J = 8.1, 9.0 Hz, 1H), 6.45 (q, J = 6.9 Hz, 1H), 2.91 (s, 3H), 1.84 (d, J = 6.9 Hz, 3H).

With the rapid development of chemical substances, we look forward to future research findings about 756520-66-8.

Reference:
Article; Zhang, Dengyou; Zhang, Xiaowei; Ai, Jing; Zhai, Yun; Liang, Zhongjie; Wang, Ying; Chen, Yi; Li, Chunpu; Zhao, Fei; Jiang, Hualiang; Geng, Meiyu; Luo, Cheng; Liu, Hong; Bioorganic and Medicinal Chemistry; vol. 21; 21; (2013); p. 6804 – 6820;,
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Related Products of 4415-82-1 , The common heterocyclic compound, 4415-82-1, name is Cyclobutylmethanol, molecular formula is C5H10O, 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.

Example 62A 3-(Cyclobutyloxy)pyridine hydrochloride With ice cooling, 2.59 g (13.7 mmol) of triphenylphosphine were added to a solution of 1.00 g (10.5 mmol) of 3-hydroxypyridine and 1.3 ml (13.7 mmol) of cyclobutylmethanol in 20 ml of THF, and the mixture was stirred for 5 min. 2.7 ml (13.7 mmol) of diisopropyl azodicarboxylate were then added dropwise and the reaction mixture was warmed to RT overnight. For work-up, water was added and the mixture was extracted twice with in each case 50 ml of ethyl acetate. The combined organic phases were washed with saturated sodium chloride solution, dried over magnesium sulphate and concentrated. The crude product was stirred with 50 ml of cyclohexane and the white solid was filtered off with suction and washed three times with in each case 20 ml of cyclohexane. The filtrate was concentrated and dissolved in 40 ml of diethyl ether, and 3 ml (12 mmol) of a 4N solution of hydrogen chloride in dioxane were added with ice cooling. The resulting beige precipitate was filtered off, washed twice with in each case 20 ml of diethyl ether and dried under HV. This gave 1.67 g (76% of theory) of the target compound. LC-MS [Method 10]: Rt=1.46 min; MS (ESIpos): m/z=164 (M+H)+ 1H-NMR (400 MHz, DMSO-d6): delta [ppm]=1.77-2.01 (m, 4H), 2.03-2.17 (m, 2H), 2.68-2.84 (m, 1H), 4.19 (d, 2H), 7.90 (dd, 1H), 8.10 (dd, 1H), 8.47 (d, 1H), 8.65 (d, 1H).

The synthetic route of 4415-82-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Bayer Pharma Aktiengesellschaft; BECKER-PELSTER, Eva Maria; BUCHGRABER, Philipp; BUCHMUeLLER, Anja; ENGEL, Karen; GNOTH, Mark Jean; HIMMEL, Herbert; KAST, Raimund; KELDENICH, Joerg; KLAR, Juergen; KNORR, Andreas; LANG, Dieter; LINDNER, Niels; SCHMECK, Carsten; SCHOHE-LOOP, Rudolf; TINEL, Hanna; TRUeBEL, Hubert; WUNDER, Frank; (97 pag.)US2016/318866; (2016); A1;,
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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. 307353-32-8, name is Methyl 3-bromo-5-(hydroxymethyl)benzoate, the common compound, a new synthetic route is introduced below. Recommanded Product: 307353-32-8

TBDPS-Cl (15.9 mL, 16.8 g, 61.21 mmol) was added to a solution of methyl 3-bromo-5-(hydroxymethyl)benzoate (10 g, 40.8 mmol) in CH2Cl2 (408 mL) at 23 C. and stirred for 1 h. The resultant heterogeneous reaction mixture was filtered and concentrated in vacuo. The residue was purified by flash chromatography (Combi-flash Rf, Hex/EtOAc=0-10% gradient) to afford the title compound (18.2 g, 37.6 mmol, 92%) as a white solid. 1H NMR (400 MHz, Chloroform-d) delta 8.05 (s, 1H), 7.89 (s, 1H), 7.76-7.64 (m, 5H), 7.48-7.34 (m, 6H), 4.75 (s, 2H), 3.91 (s, 3H), 1.11 (s, 9H).

The synthetic route of 307353-32-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Vanderbilt University; Alvarado, Joseph R.; Stauffer, Shaun R.; Gogliotti, Rocco D.; Han, Changho; Meyers, Kenneth M.; Tian, Jianhua; Macdonald, Jonathan D.; Fesik, Stephen W.; Lee, Taekyu; US2020/102288; (2020); A1;,
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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. 445-26-1, name is 1-(2-Fluorophenyl)ethanol, the common compound, a new synthetic route is introduced below. name: 1-(2-Fluorophenyl)ethanol

Step 1: 5-(4-Bromo-phenyl)-3-methyl-isoxazole-4-carboxylic acid (4 g, 14.2 mmol) was dissolved in toluene (150 mL). Triethylamine (2.187 mL, 15.6 mmol) was added, followed by diphenylphosphoryl azide (3.372 mL, 15.6 mmol), and the mixture was stirred for 10 minutes. 2-Fluoro-alpha-methylbenzyl alcohol (2 g, 15.6 mmol) was added, and the reaction was stirred at 80 C. overnight. The mixture was cooled to room temperature and concentrated, and the residue was partitioned between with EtOAc and water. The organic layer was washed 4 times with water and once with brine, and then dried, filtered, and concentrated, and the residue was purified by silica gel chromatography (dry load; 0-100% EtOAc in hexanes) to give [5-(4-bromo-phenyl)-3-methyl-isoxazol-4-yl]-carbamic acid 1-(2-fluoro-phenyl)-ethyl ester.

The synthetic route of 445-26-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; AMIRA PHARMACEUTICALS, INC.; US2010/152257; (2010); A1;,
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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.4845-50-5, name is 1,4-Dioxane-2,3-diol, molecular formula is C4H8O4, molecular weight is 120.1039, as common compound, the synthetic route is as follows.SDS of cas: 4845-50-5

3.91 g (17.532 mmol) of the compound from example 96A was dissolved in 230 ml ethanol, 2.85 g (22.768 mmol) of 2,3-dihydroxy-l,4-dioxane was added and it was stirred overnight at room temperature. The reaction mixture was concentrated in a rotary evaporator, wherein the product crystallized out. It was cooled with ice water, the product was filtered off and dried under vacuum. We obtained 3.04 g (71% of theor.) of the target compound.LC-MS (method 10): R, = 0.92 min; MS (EIpos): m/z = 245 [M+H]+. 1H-NMR (400 MHz, DMSO-D6): delta [ppm] = 8.46 (dd, IH), 9.06-9.09 (m, 2H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,4845-50-5, 1,4-Dioxane-2,3-diol, and friends who are interested can also refer to it.

Reference:
Patent; BAYER SCHERING PHARMA AKTIENGESELLSCHAFT; BAeRFACKER, Lars; KAST, Raimund; GRIEBENOW, Nils; MEIER, Heinrich; KOLKHOF, Peter; ALBRECHT-KUePPER, Barbara; NITSCHE, Adam; STASCH, Johannes-Peter; SCHNEIDER, Dirk; TEUSCH, Nicole; RUDOLPH, Joachim; WHELAN, James; BULLOCK, William; PLEASIC-WILLIAMS, Susan; WO2010/20363; (2010); A1;,
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Application of 52273-77-5, 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.52273-77-5, name is 2-(3-Aminophenyl)ethanol, molecular formula is C8H11NO, molecular weight is 137.179, as common compound, the synthetic route is as follows.

Step 1. Preparation of 3-{2-[2-(4-tert-Butyl-phenyl)-thiazol-4-ylmethoxy]-ethyl}-phenyl amine To a solution of 0.027 g (1 mmol) of 95% sodium hydride and 0.5 drop of 15-crown-5 in 20 mL of THF was added dropwise a solution of 0.139 g (1 mmol) of 3-(2-hydroxy ethyl) phenyl amine at 0 C. After stirring for 0.5 hr 0.28 g (1.1 mmol) of 4-chloromethyl-2-(4-tert-butyl phenyl) thiazole was added in one portion. The mixture was stirred at room temperature for 5 hr. At the end of this time, the solution was concentrated and the residue washed with 10 ml of saturated ammonium chloride and extracted 2 times with 30 mL of ethyl acetate. The organic layers were combined, dried (MgSO4) and concentrated to recover an oil, which was purified by column chromatography on SiO2 with 30% ethyl acetate: hexane elution to provide 0.125 g of product as an oil, used in the next step without further purification. NMR (400 MHz, DMSO-d6) delta7.83 (d, J=8 Hz,2H, ArH), 7.50 (d, J=8 Hz, 2H,ArH), 7.45 (s, 1H, N=CH) 7.08 (t, J=8 Hz, 1H, H5), 6.63 (d, J=8 Hz, 1H,H4), 6.54 (s, 1H, H2), 6.51 (d, J=8 Hz, 1H, H6) 4.59 (s, 2H, OCH2), 3.71 (t, J=7 Hz, 2H, OCH2), 2.87 (t, J=7 Hz, 2H,ArCH2), 1.30 (s, 9H, t-bu)

Statistics shows that 52273-77-5 is playing an increasingly important role. we look forward to future research findings about 2-(3-Aminophenyl)ethanol.

Reference:
Patent; Wyeth; US2003/203941; (2003); A1;,
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