Month: July 2021

Adding a certain compound to certain chemical reactions, such as: 7287-82-3, 1-(2-Methylphenyl)ethanol, 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, Safety of 1-(2-Methylphenyl)ethanol, blongs to alcohols-buliding-blocks compound. Safety of 1-(2-Methylphenyl)ethanol

General procedure: In a typical process, into a 5ml two-necked, round-bottom flask equipped with a magnetic stirrer and a thermometer were added the ruthenium complex [Ru(pymieb)(pydic)] (0.002mmol) and the substrate alcohol (2mmol) successively. The mixture was heated to 40C under stirring. Then t-butyl hydroperoxide (TBHP) was added dropwise to the mixture and the temperature was kept at 40C until completion of the reaction. The reaction samples were analyzed on a Shandong Lunan Ruihong Gas Chromatograph (SP-6800A) equipped with a FID detector and a SE 30 column (30m×0.5mm). The conditions used in gas chromatography were temperature of the detector 280C, column temperature 130-220C (varying with alcohols), pressure of the carrier gas 0.05-0.07MPa (varying with alcohols).

The synthetic route of 7287-82-3 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Zhang, Yuecheng; Liu, Liu; Cao, Xiaohui; Zhao, Jiquan; Polyhedron; vol. 105; (2016); p. 170 – 177;,
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Electric Literature of 62058-03-1, 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. 62058-03-1, name is trans-4-Aminoadamantan-1-ol, molecular formula is C10H17NO, 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.

Example B .4 a) Preparation of compound 4; A mixture of 2-[(4-chlorophenyl)thio]-2-methylpropanoic acid [17413-74-0] (0.0007 mol) in dichloromethane (5 ml), DMF (5 ml) and DIPEA (0.5 ml) was stirred and l-[bis(dimethylamino)methylene]-lH-benzotriazolium, hexafluorophosphate(l-), 3-oxide (EtaBTU)(0.0075 mol) was added. After stirring for 15 minutes (lalpha,3alpha,4alpha,5beta,7alpha) -4-aminotricyclo[3.3.1.13’7]decan-l-ol [62058-03-1] (0.00075 mol) was added. The reaction mixture was stirred overnight at 40°C and the solvent was evaporated. The residue was dissolved in dichloromethane and then the solution was washed with a 15 percent citric acid solution and with a sodium carbonate solution. The organic layer was separated, dried, filtered off and the solvent was evaporated. The obtained residue was purified by column chromatography over silica gel (Supelco) (eluent: dichloromethane). The product fractions were collected and the solvent was evaporated, yielding 0.164 g of compound 4.

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 62058-03-1, trans-4-Aminoadamantan-1-ol.

Reference:
Patent; JANSSEN PHARMACEUTICA N.V.; WO2006/24627; (2006); A2;,
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Reference of 10488-69-4, Adding some certain compound to certain chemical reactions, such as: 10488-69-4, name is Ethyl 4-chloro-3-hydroxybutanoate,molecular formula is C6H11ClO3, 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 10488-69-4.

Example 1 Preparation of (S)-Ethyl-3-hydroxy-4-(1-phenyl-1H-tetrazol-5-ylthio)butanoate (11a) 121.2 g of triethylamine and 100 g of (S)-4-chloro-3-hydroxybutyric acid ester were added to the solution of 96.2 g of 1-phenyl-1H-terazole-5-thiol in 750 mL toluene at 25° C. The reaction mixture was heated to 80° C. to 85° C. for completion of reaction on TLC. The reaction mixture was cooled to 25° C. and treated with 200 mL of water and stirred to separate the layers. The separated aqueous layer was twice extracted with 100 mL toluene. The combined organic layer was treated with 300 mL HCl solution followed by washing with 200 ml water. The organic layer was distilled under vacuum below 50° C. The residue was treated with 200 ml hexane and stirred for 30 minutes. The solution was distilled under vacuum below 50° C. to remove hexane and obtain (S)-Ethyl-3-hydroxy-4-(1-phenyl-1H-tetrazol-5-ylthio)butanoate (11a) as an oil.

According to the analysis of related databases, 10488-69-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Dwivedi, Shriprakash Dhar; Patel, Dhimant Jasubhai; Rupapara, Mahesh Laljibhai; US2013/158263; (2013); A1;,
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Reference of 623-50-7 ,Some common heterocyclic compound, 623-50-7, molecular formula is C4H8O3, 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.

1 (100.0 g, 960.52 mmol) and imidazole (77.3 g, 1.15 mol)Soluble in dichloromethane (1.5L),Under an ice bath, tert-butyldiphenylchlorosilane (264.0 g, 960.52 mmol) was slowly added dropwise using a constant pressure dropping funnel.After the addition is completed,Transfer to room temperature for 16 h.filter,The filtrate was washed with a 1.0 mol/L hydrochloric acid solution (300 ml × 2).The dichloromethane layer was washed with a saturated sodium bicarbonate solution (100 ml x 2).Dry over anhydrous sodium sulfate,Concentrated to a white clear liquid 2 (297.7 g, 91%).

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. 623-50-7, Ethyl 2-hydroxyacetate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Guangzhou Yue Mei Pharmaceutical Technology Co., Ltd.; Guo Zhongwu; Hao Linghua; Zhong Bohua; Zheng Junxia; (10 pag.)CN108997429; (2018); A;,
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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. 55489-58-2, name is 2-(2-(2-(Benzyloxy)ethoxy)ethoxy)ethanol, molecular formula is C13H20O4, 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. HPLC of Formula: C13H20O4

15-Bromo-1 -phenyl-2,5,8,11-tetraoxapentadecane To a suspension of sodium hydride, 60 % w/w in mineral oil (0.250 g, 6.24 mmol) in DMF (2 mL) was added a solution of 2-(2-(2-(benzyloxy)ethoxy)ethoxy)ethanol (1 g, 4.16 mmol) (commercially available from for example Fluorochem) in DMF (2 mL) at 0 C. After stirring for 25 minutes, 1,4-dibromobutane (commercially available from for example Aldrich) (4.04 g, 18.73 mmol) dissolved in DMF (2 mL) was added dropwise to the mixture. The reaction was stirred under an atmosphere of nitrogen for 2.5 hours. A further aliquot of sodium hydride, 60 % w/w in mineral oil (0.250 g, 6.24 mmol) was added and the reaction was stirred at 0 C for 30 minutes. The reaction was warmed to room temperature and stirred for 30 minutes. A final aliquot of sodium hydride, 60 % w/w in mineral oil (0.250 g, 6.24 mmol) was added and the reaction stirred at room temperature for 2 hours then left standing over the weekend. The reaction mixture was filtered through celite and the solid washed with DCM. The filtrate was partitioned between DCM (30 mL) and water (30 mL). The organic extract was washed with brine (2 x 30 mL), dried using a hydrophobic frit and concentrated under reduced pressure. The product was purified by chromatography on silica using a gradient elution from 0% to 100% methyl tert-butyl ether in cyclohexane to afford the title compound (711 mg, 1.89 mmol, 46% yield). LCMS RT= 1.16 min, ES+ve m/z 375.2/377.1 [M+H]+.

With the rapid development of chemical substances, we look forward to future research findings about 55489-58-2.

Reference:
Patent; YALE UNIVERSITY; GLAXOSMITHKLINE INTELLECTUAL PROPERTY DEVELOPMENT LIMITED; CAMBRIDGE ENTERPRISE LIMITED UNIVERSITY OF CAMBRIDGE; CREWS, Craig, M.; BUCKLEY, Dennis; CIULLI, Alessio; JORGENSEN, William; GAREISS, Peter, C.; MOLLE, Inge, Van; GUSTAFSON, Jeffrey; TAE, Hyun-Seop; MICHEL, Julien; HOYER, Dentin, Wade; ROTH, Anke, G.; HARLING, John, David; SMITH, Ian Edward, David; MIAH, Afjal, Hussain; CAMPOS, Sebastian, Andre; LE, Joelle; WO2013/106646; (2013); A2;,
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Adding a certain compound to certain chemical reactions, such as: 767-90-8, (2-Ethylphenyl)methanol, 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, 767-90-8, blongs to alcohols-buliding-blocks compound. Recommanded Product: 767-90-8

Step 1: A solution of (2-ethylphenyl)methanol (500 mg, 3.67 mmol) and triethylamine (742 mg, 7.34 mmol) in DCM (5 mL) was added MsCI (1.0 g, 8.73 mmol) at 000 and stirred at 000 for 0.5 hour. Then it was stirred at 20C for 1 hour. The mixture was quenched with water (0.5 mL), and diluted with DCM (10 mL). The mixture was added NaHCO3 (aq.) until pH=8. The organic layer was washed with water (3 x 5 mL), dried with an hydrous Na2504, filteredand concentrated under vacuum to give 2-ethylbenzyl methanesulfonate (600 mg), which was used into the next step 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,767-90-8, its application will become more common.

Reference:
Patent; H. LUNDBECK A/S; KEHLER, Jan; RASMUSSEN, Lars, Kyhn; LANGGARD, Morten; JESSING, Mikkel; VITAL, Paulo, Jorge, Vieira; JUHL, Karsten; (159 pag.)WO2016/174188; (2016); 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. 10488-69-4, name is Ethyl 4-chloro-3-hydroxybutanoate, molecular formula is C6H11ClO3, 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. Quality Control of Ethyl 4-chloro-3-hydroxybutanoate

To 1 L of a 3-necked round bottom flask equipped with a thermometer, a pH meter and a stirrer, 64.8 g of glycinamide hydrochloride, 98.5 g of sodium bicarbonate and 500 mL of ethyl alcohol were successively added and stirred at a room temperature for 1 hour. To the solution, 97.7 g of ethyl- (S)-4-chloro-3-hydroxybutyric was dropwisely added. The reaction solution was further stirred at 80°C for 20 hours. Work-up procedures were performed in the same manner as mentioned in the Example 7. Recrystallization with methyl alcohol and acetone gave 52.5 g of the targeted (S)-4-hydroxy-2-oxo- I -pyrrolidine acetamide.

With the rapid development of chemical substances, we look forward to future research findings about 10488-69-4.

Reference:
Patent; AHN-GOOK PHARMACEUTICAL CO., LTD.; RSTECH CORPORATION; WO2005/115978; (2005); A1;,
Alcohol – Wikipedia,
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Synthetic Route of 597-31-9, 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. 597-31-9, name is 3-Hydroxy-2,2-dimethylpropanal, molecular formula is C5H10O2, 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.

Test SetupThe liquid phase hydrogenation was effected over a commercial supported nickel catalyst in the tubular reactor in liquid phase mode. The catalyst volume was 1.8 liters. The hydroxypivalaldehyde-containing crude aldol addition product and hydrogen were supplied continuously at the bottom of the tubular reactor. The hydrogenated material was withdrawn via the top of the tubular reactor, passed into a high-pressure separator and conducted out of the latter by means of level control into an ambient pressure reservoir. The hydrogenation temperature, the hydrogen pressure and the catalyst hourly space velocity were adjusted according to the conditions of the tables which follow. The crude hydroxypivalaldehyde-containing aldol addition product used for the hydrogenation tests had the following typical composition.Organic component (determined by gas chromatography, data in percent): In the analysis data given below for the starting streams, the critical contents for the aliphatic alcohols serving as diluents and the water content were reported. In the analysis of the hydrogenation outputs, the residual contents of HPA and of ester compounds and the NPG content were stated.Liquid phase hydrogenation of HPA at a hydrogenation temperature of 130 C.As a comparison of the test data shows, the proportion of the desired NPG in the hydrogenation output also increases with rising water content in the starting mixture. When, for example, proceeding from test 3, the water content is established below the critical limit of 15% by weight (comparative test 5), the NPG content in the hydrogenation output is lowered. This development is also manifested in tests 6, 7, and 8 (comparative), in which the content of NPG in the hydrogenation output likewise decreases with falling water content in the starting material. The pressure selected in comparative example 9 is no longer sufficient for a satisfactory HPA conversion.

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

Reference:
Patent; Schalapski, Kurt; Kretz, Tonia; Kreickmann, Thosrten; Heymanns, Peter; Lukas, Rainer; Schulz, Rolf-Peter; US2011/98515; (2011); A1;,
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Synthetic Route of 53463-68-6, 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 53463-68-6, name is 10-Bromodecanol. This compound has unique chemical properties. The synthetic route is as follows.

(10-Bromo-decyloxy)-t-butyl-dimethyl-silane. To a stirred solution of 10-bromo- decanol (2.44 g, 10.3 mmol) in NMP (13 mL) at 0 C, TBSCI (1.66 g, 11.0 mmol) was added followed by imidazole (0,716 g, 10,5 mmol) portion wise (3 x 0,200 g & 1 x 0,116 g) in 15 min intervals. After the last portion of imidazole had been added, the reaction was stirred for an additional 2 h at 0 C and then it was poured into water (100 mL). The product was extracted into pentane (100 mL), the’organic phase-was concentrated/7 ? vacuo (20 mbar, 50 C) and the crude liquid was purified by filtration through a short silica gel column, using 1: 9 MTBE : petroleum benzene as eluent. The product was obtained as a colorless liquid (3.12 g, 8. 88 mmol, 86% yield based on 10-bromo-decan-1-ol). Reaction conditions were not optimized.

According to the analysis of related databases, 53463-68-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; DSM IP Assets B.V.; WO2005/47223; (2005); A1;,
Alcohol – Wikipedia,
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Related Products of 67853-03-6, 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 67853-03-6, name is Methyl 3-(hydroxymethyl)benzoate. This compound has unique chemical properties. The synthetic route is as follows.

General procedure: In a plastic reaction vessel equipped with a Teflon-coated magnetic stiffer was charged DEOXO-FLUOR (6 eq., 2.7 M solution in toluene). To this was then added sequentially 3-acetyl-benzoic acid methyl ester (1 eq.) and ethanol (1 eq.), and the resulting mixture was heated at 85C for 3 days. The reaction mixture was then cooled to RT, diluted with EtOAc and washed with brine. The organic extract was then dried over MgSO4, filtered and the filtrate concentrated in vacuo. Purification of the residue thus obtained by way of column chromatography (Si02, gradient elution, Hex -> 9:1 (v/v) Hex: EtOAc) afforded the intermediate ester as a colorless oil. This was then immediately taken up in methanol (0.1 M), added lithium hydroxide (1 eq.) and then stirred at RT for 16 h. The resulting reaction mixture was carefully neutralized with HC1 (4 M in dioxane) and the volatiles were removed in vacuo. The resulting residue was subjected to column chromatography (Si02, gradient elution, 9:1 (v/v) Hex: EtOAc-> EtOAc) to furnish the desired product as a white solid (68% yield). Prepared in an analogous fashion to Intermediate acid 4, but using 3- hydroxymethyl-benzoic acid methyl ester (1 eq.) in place of 3-acetyl-benzoic acid methyl ester and DAST (1.5 eq.) in place of DEOXO-FLUOR. Furthermore, the reaction took place at -78C over 1 h instead of 85C over 3 days (14% yield).

According to the analysis of related databases, 67853-03-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; MERCK PATENT GMBH; JORAND-LEBRUN, Catherine; LAN, Ruoxi; CHEN, Austin; CLARK, Ryan C.; (268 pag.)WO2017/49068; (2017); A1;,
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