Month: March 2021

Reference of 69605-90-9, 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. 69605-90-9, name is [1,1′-Biphenyl]-3-ylmethanol. A new synthetic method of this compound is introduced below.

General procedure: Oxidation of alcohols was typically carried out as follows: a suspension with 5 mg of the synthesized catalyst in acetonitrile (2 mL) was magnetically stirred, and the substrate namely alcohols (0.1 mmol) and PhIO (2.5 equiv.) was then added. The resulting mixture was kept at 60 C with magnetical stirring for a set time. The selectivity and conversion were determined by GC analysis.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,69605-90-9, its application will become more common.

Reference:
Article; Yang, Zhi-Wang; Zhao, Xia; Li, Tian-Jing; Chen, Wen-Long; Kang, Qiao-Xiang; Xu, Xue-Qing; Liang, Xi-Xi; Feng, Ying; Duan, Huan-Huan; Lei, Zi-Qiang; Catalysis Communications; vol. 65; (2015); p. 34 – 40;,
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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. 6214-44-4, name is (4-Ethoxyphenyl)methanol, the common compound, a new synthetic route is introduced below. Computed Properties of C9H12O2

To a solution of (4-ethoxyphenyl)methanol (300 mg, 1.971 mmol, commercial source: Apollo SCI) and triethylamine (328 muIota_, 2.365 mmol) in Dichloromethane (15 mL) at 0C, methanesulfonyl chloride (168 muIota_, 2.168 mmol) was added dropwise. The mixture was stirred at 0 C for 3 h. Upon completion, the reaction mixture was diluted with water and DCM and extracted with DCM (2x20ml). The combined organic layers were dried over anh. MgS04 and filtered. The filtrate was concentrated under reduced pressure to obtain 4-ethoxybenzyl methanesulfonate (454 mg, 100%) This product was used without any purification in the next reaction.

The synthetic route of 6214-44-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GLAXOSMITHKLINE INTELLECTUAL PROPERTY DEVELOPMENT LIMITED; ALEMPARTE-GALLARDO, Carlos; ENCINAS, Lourdes; ESQUIVIAS PROVENCIO, Jorge; (206 pag.)WO2019/34729; (2019); A1;,
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Adding a certain compound to certain chemical reactions, such as: 5259-98-3, 5-Chloropentan-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, COA of Formula: C5H11ClO, blongs to alcohols-buliding-blocks compound. COA of Formula: C5H11ClO

Intermediate 1; 4-(5-Chloro-pentyloxy)-benzoic acid methyl ester; 4-Hydroxy-benzoic acid methyl ester (1.52 g, 10 mmol), 5-chloro-l-pentanol (1.22 g, 10 mmol) and triphenylphosphine (2.62 g, 10 mmol) are dissolved in dry THF (30 rnL) and cooled to 0 0C. Diethylazodicarboxylate (DEAD) (1.74 g, 10 mmol) is dropped into this mixture at 0 ¡ãC and stirred at room temperature for 3 days. The reaction mixture is washed with brine, dried over Na2SO4, filtered and evaporated. The crude product is purified using silica-gel column chromatography (CH2CI2 only to CH2Cl2:2 M NH3 in MeOH=20:l) to give the desired product (1.14 g, 45percent). NMR (CDCI3): delta 7.98 (d, 2H , J = 8.8 Hz), 6.89 (d, 2H, / = 8.8Hz), 4.02 (t, 2H, J = 6.5 Hz), 3.88 (s, 3H), 3.57 (t, 2H, / = 6.7 Hz), 1.85 (m, 4H), 1.64 (m, 2H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,5259-98-3, 5-Chloropentan-1-ol, and friends who are interested can also refer to it.

Reference:
Patent; ELI LILLY AND COMPANY; WO2006/101808; (2006); A1;,
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Reference of 2077-19-2 ,Some common heterocyclic compound, 2077-19-2, molecular formula is C9H11BrO, 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 Palladium Mediated Coupling Procedure; The following general procedure illustrates the method used for Pd mediated N-arylation of the pyrrolidin-2-one moiety with the corresponding aryl bromide: To a sealed tube was added 3- [5-fluoro-2- (4-methyl-piperazin-1-yl)-benzyl]-pyrrolidin-2-one (Preparation 13), aryl bromide (1.2 equiv), dipalladium tris (dibenzylideneacetone) (0.05 equiv), 9, 9-dimethyl-4, 5- bis (diphenylphosphino) xanthene (XANTPHOS) (0.15 equiv), cesium carbonate (1.5 equiv), and dioxane (7 volumes). The mixture was heated at 100 C for 12 to 24 hours. After cooling to room temperature, the mixture was concentrated in vacuo and was purified by silica gel chromatography. The following compounds were prepared via the general procedure above:; Example 1; 3-r5-Fluoro-2-(4-methyl-piperazin-1-vl)-benzvil-1-14-(1-hvdroxv-1-methyl-ethyl)-phenvll-pyrrol idin- 2-one:; 3- [5-Fluoro-2- (4-methyl-piperazin-1-yl)-benzyl]-1- [4- (1-hydroxy-1-methyl-ethyl)-phenyl]- pyrrolidin-2-one : 13C NMR (100 MHz, CDCI3) d 24.8, 31.9, 32. 5, 44. 7, 46.0, 46.9, 52.9, 55.7, 72.4, 113.9, 114.1, 116.8, 117.1, 119.7, 1222.4, 122.5, 125.2, 137.8, 137. 9, 138.2, 145.6, 147. 9, 158. 6, 161.1, 175.5 ; MS (AP/CI) 426.3 (M+H) +. The enantiomers were separable by HPLC (90/10 heptane/ethanol ; Chiralcel OD, 10 cm x 50 cm; 275 mL/minute). Approximate retention times: t1 = 12.7 minutes; t2 = 14.8 minutes

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. 2077-19-2, 2-(4-Bromophenyl)propan-2-ol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; PFIZER PRODUCTS INC.; WO2005/90300; (2005); A1;,
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Related Products of 431-38-9, 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.431-38-9, name is 3-Amino-1,1,1-trifluoropropan-2-ol, molecular formula is C3H6F3NO, molecular weight is 129.0811, as common compound, the synthetic route is as follows.

3-Oxo-2-(pyridin-3-yl)-6-[4-(trifluoromethyl)phenyl]-2 ,3-di hydropyridazi ne-4-carboxylic acid (100 mg, 0.277 mmcl) was dissolved in anhydrous DMF (2.1 mL). (2RS)-3-Amino-1,1,1- trifluoropropan-2-ol (71.5 mg, 0.55 mmol), N-ethyl-N-isopropylpropan-2-amine (314 pL, 1.80mmol), and propane phosphonic acid anhydride (T3P, 243 pL, 50% in DMF, 415 pmol) were successively added. It was stirred at rt overnight. The reaction mixture was diluted with dichloromethane and concentrated under vacuum. The residue was purified by RP-HPLC (column: X-Bridge 018 5pm lOOx3Omm, mobile phase: (water + 0.2 vol% aqueous ammonia (32%)) acetonitrile, gradient) yielding 57.3 mg (44%) of the title compound.1H-NMR (400MHz, DMSO-d6): 6 [ppm] = 3.49 (ddd, 1H), 3.76 (ddd, 1H), 4.18-4.29 (m, 1H),6.68 (br s, 1H), 7.65 (ddd, 1H), 7.89 (d, 2H), 8.18 (ddd, 1H), 8.22 (d, 2H), 8.71 (dd, 1H), 8.75(s, 1H), 8.93 (d, 1H), 9.59 (t, 1H).

Statistics shows that 431-38-9 is playing an increasingly important role. we look forward to future research findings about 3-Amino-1,1,1-trifluoropropan-2-ol.

Reference:
Patent; BAYER AKTIENGESELLSCHAFT; BAYER PHARMA AKTIENGESELLSCHAFT; DEUTSCHES KREBSFORSCHUNGSZENTRUM; GUTCHER, Ilona; ROeHN, Ulrike; SCHMEES, Norbert; ZORN, Ludwig; ROeSE, Lars; BADER, Benjamin; KOBER, Christina; CARRETERO, Rafael; STOeCKIGT, Detlef; IRLBACHER, Horst; PLATTEN, Michael; (397 pag.)WO2018/146010; (2018); 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.702-98-7, name is 2-Methyladamantan-2-ol, molecular formula is C11H18O, molecular weight is 166.26, as common compound, the synthetic route is as follows.Recommanded Product: 702-98-7

A reactor made of glass was charged with 160 g of n-undecane, 80 g of 2-methyladamantanol, 4.1 g of methacrylic acid and 0.92 g of p-toluenesulfonic monohydrate. The resulting mixture was maintained for 1 hour while distilling off water under atmospheric pressure. Water was removed further by reflux at 120 C. for 1 hour under reduced pressure at 150 mmHg, whereby 2-methyladamantane was prepared. It was cooled to 0 C. A methacrylate forming reaction was then carried out by adding 103.6 g of methacrylic acid and 13.7 g of boron trifluoride ethyl ether to it while stirring the resulting mixture for 2 hours. After the reaction mixture was washed with 1275.5 g of a 10% aqueous sodium carbonate solution, followed by washing three times with 160 g of deionized water. In such a manner, 260 g of a n-undecane solution of 2-methyladamantan-2-yl methacrylate was obtained. The resulting solution contained 29.6 wt. % of 2-methyladamantan-2-yl methacrylate and 5.2 wt. % of 2-methyleneadamantane. The present invention was described specifically by using specific modes. It is however apparent for those skilled in the art that the present invention can be changed or modified without departing from the gist and scope of the present invention.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,702-98-7, 2-Methyladamantan-2-ol, and friends who are interested can also refer to it.

Reference:
Patent; Mitsubishi Chemical Corporation; US2008/51597; (2008); A1;,
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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. 2240-88-2, name is 3,3,3-Trifluoropropan-1-ol, molecular formula is C3H5F3O, 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. Formula: C3H5F3O

Intermediate 31 3f3-trifluoropropoxy)methyl)pyrimidine To a solution of (2-chloro-6-(l-ethoxyvinyl)pyrimidin-4-yl)methyl methanesulfonate (0.452 g, 1.54 mmol) in benzene (7 mL) were added 3,3,3-trifluoropropan-l-ol (0.264 g, 2.32 mmol), sodium hydroxide (5 M, 0.463 mL, 2.32 mmol) and tetrabutylammonium hydrogen sulfate (0.052 g, 0.15 mmol). The mixture was stirred vigourously over night at room temperature. The mixture was filtered through a short silica plug with magnesium sulfate on top. The filter was washed with EtOAc. The mixture was purified by preparative HPLC to give 2-chloro-4-(l- ethoxyvinyl)-6-((3,3,3-trifluoropropoxy)methyl)pyrimidine 0.055 g 11 percent). MS (ES+) m/z 311 [M+H]+.

With the rapid development of chemical substances, we look forward to future research findings about 2240-88-2.

Reference:
Patent; ACTURUM LIFE SCIENCE AB; BESIDSKI, Yevgeni; YNGVE, Ulrika; PAULSEN, Kim; LINDE, Christian; MACSARI, Istvan; MALMBORG, Jonas; PAPTCHIKHINE, Alexander; ARVIDSSON, Per; WO2014/195323; (2014); 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. 10029-04-6, name is Ethyl 2-(hydroxymethyl)acrylate. A new synthetic method of this compound is introduced below., name: Ethyl 2-(hydroxymethyl)acrylate

General procedure: To a solution of the appropriate allylic alcohol 6 (1.00 equiv.) in dichloromethane (0.1 M) was added vinyl acetic acid 7 (1.20 equiv.), dicyclohexylcarbodiimide (1.20 equiv.) and 4-N,N-dimethylaminopyridine (0.15 equiv.) at 0C. The mixture was allowed to warm to ambient temperature and stirred until the product was fully converted (TLC). The solution was filtered and the filter cake was washed three times with dichloromethane. The combined organic layers were washed with aq. HCl (1 M) and then with saturated aq. NaHCO3 solution, dried with Na2SO4, filtered and dry-loaded on silica gel. The pure product was obtained after column chromatography on silica, using hexane/MTBE mixtures of increasing polarity as eluents.

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, 10029-04-6, Ethyl 2-(hydroxymethyl)acrylate.

Reference:
Article; Schmidt, Bernd; Audoersch, Stephan; Kunz, Oliver; Synthesis; vol. 48; 24; (2016); p. 4509 – 4518;,
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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. 597-31-9, name is 3-Hydroxy-2,2-dimethylpropanal. This compound has unique chemical properties. The synthetic route is as follows. Application In Synthesis of 3-Hydroxy-2,2-dimethylpropanal

Hydrogenation; The starting solution used was the mixture described above as hydrogenation feed. From 0 to 7% by weight (based on the hydrogenation feed) of a 15% by weight aqueous solution of trimethylamine (from 2 to 5% by weight (based on the hydrogenation feed), or of a 5% by weight aqueous solution of citric acid in the comparative examples) were added to this mixture in order to establish the particular pH of the hydrogenation effluent specified in Table 1. The hydrogenation feed thus obtained was pumped over the catalyst in a hydrogenation reactor with liquid circulation (circulation:feed=10:1) with a catalyst hourly space velocity of 0.4 kgHPA/Icat¡Áh in trickle mode at 40 bar and 120 C.A comparison of the process according to the invention with comparative examples V1 and V2, in which the pH of the hydrogenation effluent is in each case outside the inventive range, is shown by Table 1.For pH measurement, a Knick model 766 pH meter with a Schott N1041A glass electrode was used.

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, 597-31-9, 3-Hydroxy-2,2-dimethylpropanal.

Reference:
Patent; BASF SE; US2009/69604; (2009); 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. 145691-59-4, name is (3,5-Dibromophenyl)methanol. A new synthetic method of this compound is introduced below., Recommanded Product: 145691-59-4

Step 2: To a mixture of (3,5-dibromophenyl)methanol (1 g, 3.759 mmol, 1 equiv) and PdCI2(dppf).CH2Cl2 complex (0.21 g, 0.263 mmol, 0.07 equiv) in 10 mL of dry THF at -70 ¡ãC was added 1 M diethyl zinc in hexane (15 mL). The resulting mixture was allowed to warm to room temperature, and stirred at 45 ¡ãC for overnight. To drive the reaction to completion, additional 11.3 mL of 1 M diethyl zinc in hexane was added with continued stirring at 45 ¡ãC for overnight. After cooling, the reaction mixture was added to a stirred mixture of dilute HCI and EtOAc. Organic layer was separated, washed with water, dried over Na2S04, filtered, and concentrated in vacuo to afford crude product. The crude product was purified by flash column chromatography with silica gel cartridge using gradient elution of 0 to 10percent EtOAc in Hexane. The collected fractions with pure product were combined and concentrated in vacuo to afford (3,5-diethylphenyl)methanol as colorless liquid (0.2 g, 32percent). LC-MS (ES) m/z = 147.2 [M+H]+. H NMR (400 MHz, DMSO-d6) delta ppm 1.14 (t, J = 7.2 Hz, 6H), 2.50 – 2.56 (m, 4H), 4.41 (d, J = 5.2 Hz, 2H), 5.01 (t, J = 5.6 Hz, 1 H), 6.87 (s, 1 H), 6.93 (s, 2H).

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, 145691-59-4, (3,5-Dibromophenyl)methanol.

Reference:
Patent; GLAXOSMITHKLINE INTELLECTUAL PROPERTY (NO.2) LIMITED; AXTEN, Jeffrey Michael; FAUCHER, Nicolas Eric; DAUGAN, Alain Claude-Marie; (153 pag.)WO2017/46739; (2017); A1;,
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