Month: September 2021

Reference of 15852-73-0, 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. 15852-73-0, name is (3-Bromophenyl)methanol, molecular formula is C7H7BrO, 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: To a stirred solution of triphenylphosphine (1.5 mmol) in dry dichloromethane was added iodine (1.5 mmol)and polymer supported 4-DMAP (0.4 mmol, 40 molpercent). Stirring was continued for 2 min; alcohol (1mmol) was then added. The reaction was monitored by TLC. After complete conversion of the alcohol (as indicated byTLC), the reaction was quenched with an aqueous solution of sodium thiosulfate (20 mL). The organic solventswere removed and the aqueous solution extracted with ethylacetate (50 mL). The combined organic layers weredried using sodium sulfate (anhydrous), filtered and concentrated. The residue was purified by column chromatography (2percent EtOAc in hexane) to get the desired iodide product.

According to the analysis of related databases, 15852-73-0, the application of this compound in the production field has become more and more popular.

Reference:
Article; Das, Diparjun; H Anal, Jasha Momo; Rokhum, Lalthazuala; Journal of Chemical Sciences; vol. 128; 11; (2016); p. 1695 – 1701;,
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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. 3597-91-9, name is [1,1′-Biphenyl]-4-ylmethanol, the common compound, a new synthetic route is introduced below. Safety of [1,1′-Biphenyl]-4-ylmethanol

Synthesis of 4-(bromomethyl)biphenylCarbon tetrabromide (8.99 g) and triphenylphosphine (7.11 g) were added to a stirred solution of biphenyl-4-yl-methanol (5.00 g) in dichloromethane (100 ml) at room temperature and stirrred the reaction mixture for approximately 2 hours at the same temperature. The solvent was evaporated under reduced pressure and the residue thus obtained was purified by column chromatography using 5% diethylether in hexane as eluant to furnish the title compound (6.37 g).

The synthetic route of 3597-91-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Palle, Venkata P.; Sattigeri, Viswajanani Jitendra; Khera, Manoj Kumar; Voleti, Sreedhara Rao; Ray, Abhijit; Dastidar, Sunanda G.; US2008/194565; (2008); 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. 624-95-3, name is 3,3-Dimethylbutan-1-ol. A new synthetic method of this compound is introduced below., SDS of cas: 624-95-3

[00068] Example VI represents an oxidation in which the KBr co-catalyst and the Na2B4O7 are simultaneously present. [00069] 16.9 g of 3,3-Dimethyl-1-butanol (117.3 mmol) and 0.0765 g MeO-TEMPO (0.411 mmol) are charged in a jacketed glass reaction flask as in Example I. Sodium borate (0.380 g, 1.0 mmol) and potassium bromide (0.011 g, 0.104 mmol) are dissolved in water (12.0 cc) and the aqueous solution is added to the stirred organic fraction at 1000 RPM in the reaction flask. The stirred suspension is cooled to 0 C. and the emulsion is re-adjusted to pH 8.4 using 50% solution of CH3COOH. When the temperature of the reactants reached 0 C., 75.5 g (122 mmol) of 12.1% aqueous NaOCl solution are pumped in via a gas-tight syringe over 90 minutes (The pH of the bleach solution was adjusted to 10 using 50% aqueous CH3COOH). During the bleach addition the pH was maintained at 8.3-8.4 levels using a few drops of 50% aqueous CH3COOH. The reaction mixture is stirred for an additional 120 min at 0 C. and the organic layer is sampled for GC assay. The reaction in this second stage was kept at pH 8.4 by addition of 0.2-0.25 cc aqueous solution of NaOH (50% concentration). The yield of 3,3-dimethylbutyraldehyde is 94.0% at 60 min and 95.0% at 90 min reaction time. This yield is equivalent to the yield of Example III in which no potassium bromide 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, 624-95-3, 3,3-Dimethylbutan-1-ol.

Reference:
Patent; The NutraSweet Company; US6825384; (2004); B1;,
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Related Products of 107025-44-5 ,Some common heterocyclic compound, 107025-44-5, molecular formula is C9H18O3, 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.

To a solution of 3-iodo-1H-pyrazolo[3,4-d]pyrimidin-4-ylamine (0.626 g, 2.40 mmol) in anhydrous tetrahydrofuran (25 mL) was added triphenylphosphine (1.51 g, 5.76 mmol) and diisopropylazodicarboxylate (1.16 g, 5.76 mmol). The mixture was stirred for about five minutes at ambient temperature under a nitrogen atmosphere and 4-(2-methoxyethoxy)-cyclohexanol (JP 61229865, mixture of cis- and trans-isomers, 1.04 g, 5.98 mmol) was added. The reaction mixture was stirred at ambient temperature for about three hours. The tetrahydrofuran was removed under reduced pressure and the crude mixture was stirred in a mixture of acetone (15 mL) and aqueous hydrochloric acid (2 N, 15 mL) for two hours at ambient temperature. The acetone was removed under reduced pressure and the aqueous mixture was neutralized by the addition of saturated aqueous sodium bicarbonate solution such that the pH was approximately 8. The aqueous mixture was extracted with ethyl acetate (3×25 mL) and the combined organic fractions were dried over anhydrous magnesium sulfate. The crude mixture was purified by flash column chromatography on silica gel using ethyl acetate as the mobile phase to provide pure white solids of both trans-3-iodo-1-[4-(2-methoxyethoxy)-cyclohexyl]-1H-pyrazolo[3,4-d]pyrimidin-4-ylamine (200 mg, 0.480 mmol); 1H NMR (DMSO-d6 400 MHz) delta8.18 (s, 1H), 4.59 (m, 1H), 3.56 (dd, 2H), 3.46 (dd 2H), 3.36 (tt 1H), 3.25 (s, 3H), 2.08 (d, 2H), 1.92 (m, 4H), 1.33-1.37 (qd, 2H); m/z: (M+H)+ 418, and cis-3-iodo-1-[4-(2-methoxyethoxy)-cyclohexyl]-1H-pyrazolo[3,4-d]pyrimidin-4-ylamine (120 mg, 0.288 mmol); 1H NMR (DMSO-d6, 400 MHz) delta8.18 (s, 1H), 4.63 (tt, 1H), 3.58 (t, 1H), 3.52 (td, 2H), 3.50 (td, 2H), 3.29 (s, 3H), 2.15 (q, 2H), 1.95 (d, 2H), 1.61 (m, 4H); m/z: (M+H)+ 418

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. 107025-44-5, 4-(2-Methoxyethoxy)cyclohexanol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Wishart, Neil; Friedman, Michael; Arnold, Lee D.; Yang, Bryant; Fix-Stenzel, Shannon R.; Ericsson, Anna; Michaelides, Michael R.; Qian, Xiao-Dong; Holms, James H.; Steinman, Douglas H.; Tian, Zhengping; Wittenberger, Steven J.; US2006/25383; (2006); A1;,
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Electric Literature of 27489-62-9, 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 27489-62-9 as follows.

Compound 29 (1.15 g, 10 mmol), CBzCl (2.14 g, 12 mmol) andTEA (1.23 g, 12 mmol) were dissolved in ACN at 0-5 C and stirredfor 1 h. The reaction mixture was diluted with EtOAc and water.The organic layer was separated and washed with water (2 10mL). After drying with anhydrous Na2SO4, the organic layer wastreated with 1 g of silica gel and evaporated under reduced pressureto give a dry plug. This plug was placed on top of a silica gelcolumn and eluted with CHCl3 and MeOH. Fractions containingthe product (TLC) were pooled and evaporated to afford a whitesolid 30 in 90% yield. mp 161.6-163.8 C (lit39 163-165 C); TLCRf 0.49 (CHCl3: MeOH, 20:1); 1H NMR (CDCl3) d 1.25 (m, 2H,CH2), 1.39 (m, 2H, CH2), 1.50 (d, J = 4.00 Hz, 1H, exch, OH), 1.97(m, 4H, CH2), 3.51 (m, 1H, NCH), 3.60 (m, 1H, OCH), 4.60 (br, 1H,exch, NH), 5.10 (s, 2H, CH2), 7.38 (m, 5H, ArH); HPLC >95%; ESIMSm/z [M+H]+, calcd 250.14, found 250.22.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,27489-62-9, its application will become more common.

Reference:
Article; Xiang, Weiguo; Choudhary, Shruti; Hamel, Ernest; Mooberry, Susan L.; Gangjee, Aleem; Bioorganic and Medicinal Chemistry; vol. 26; 9; (2018); p. 2437 – 2451;,
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Adding a certain compound to certain chemical reactions, such as: 112-27-6, 2,2′-(Ethane-1,2-diylbis(oxy))diethanol, 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, 112-27-6, blongs to alcohols-buliding-blocks compound. Application In Synthesis of 2,2′-(Ethane-1,2-diylbis(oxy))diethanol

Compound triethylene glycol (5.0g, 33.3mmol) was dissolved in 10mL of dichloromethane, Et3N (6.7g, 66.6mmol) was added, TsCl (8.9g, 46.6mmol) was added dropwise under ice-dichloromethane solution. After completion of the dropwise addition, the mixture was transferred to room temperature and stirred for 12 hours. After adjusting the pH of the solution to 6 with 6M HCl, 10 mL of water was added, and the mixture was extracted three times with 30 mL of dichloromethane, and the organic phases were combined and dried over anhydrous sodium sulfate. Column chromatography (EA) gave 7.5 g of a yellow liquid product with a yield of 74%.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,112-27-6, its application will become more common.

Reference:
Patent; Hangzhou Oulian Pharmaceutical Technology Co., Ltd.; Zhang Xingxian; (22 pag.)CN109928956; (2019); A;,
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Related Products of 29683-23-6, Adding some certain compound to certain chemical reactions, such as: 29683-23-6, name is Tetrahydro-2H-thiopyran-4-ol,molecular formula is C5H10OS, 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 29683-23-6.

To a 50 mL two-neck flask were added tetrahydro-2H-thiopyran-4-ol (568 mg, 4.80 mmol) and anhydrous tetrahydrofuran (15 mL). Then p-bromophenol (530 mg, 3.00 mmol) was added at 0C, and Ph3P (1.50 g, 5.66 mmol) and diethyl azodicarboxylate (1.00 g, 5.63 mmol) were added at last. The mixture was warmed to rt and stirred for 2 h. The reaction mixture was concentrated in vacuo to remove tetrahydrofuran, and to the residue was added saturated brine (50 mL). The resulting mixture was extracted with EtOAc (30 mL*2). The combined organic layers were washed with saturated brine (30 mL*2), dried over anhydrous Na2SO4, and filtered. The filtrate was concentrated in vacuo, and the residue was purified by silica-gel column chromatography (n-hexane:EtOAc=100:1, V/V) to give a white solid (440 mg, 53.6%). 1H NMR (400 MHz, CDCl3) delta 7.39 (d, J = 8.9 Hz, 1H), 6.80 (d, J = 8.9 Hz, 1H), 4.52-4.17 (m, 1H), 3.02-2.85 (m, 1H), 2.70-2.44 (m, 1H), 2.35-2.14 (m, 1H), 2.05-2.01 (m, 1H).

According to the analysis of related databases, 29683-23-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Sunshine Lake Pharma Co., Ltd.; WANG, Xiaojun; ZHOU, Pingjian; YANG, Chuanwen; HUANG, Changwei; XIONG, Shaohui; ZHANG, Yingjun; ZHANG, Jiancun; (139 pag.)EP3342765; (2018); A1;,
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Reference of 2425-28-7, 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.2425-28-7, name is 2-Bromo-1-phenylethan-1-ol, molecular formula is C8H9BrO, molecular weight is 201.0605, as common compound, the synthetic route is as follows.

General procedure: A round-bottom flask was charged with alcohol (2 mmol), CuOTf (0.1 mmol, 0.05 equiv) (S)-5-(pyrrolidin-2-yl)-1H-tetrazole (0.1 mmol, 0.05 equiv), TEMPO (0.1 mmol, 0.05 equiv), t-BuOK (2 mmol, 1 equiv) and DMF (5 ml). The reaction mixture was stirred at 25 C open to air until the completion of the reaction, as monitored by TLC. The mixture was then diluted with CH2Cl2 (20 ml), washed with water, dried over Na2SO4, and evaporated under vacuum to give the crude product, which was purified by column chromatography to give the pure product.

The chemical industry reduces the impact on the environment during synthesis 2425-28-7, I believe this compound will play a more active role in future production and life.

Reference:
Article; Liu, Yangyang; Xie, Aming; Li, Junjian; Xu, Xiao; Dong, Wei; Wang, Boliang; Tetrahedron; vol. 70; 52; (2014); p. 9791 – 9796;,
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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. 455-01-6, name is 2-(3-(Trifluoromethyl)phenyl)ethanol. This compound has unique chemical properties. The synthetic route is as follows. HPLC of Formula: C9H9F3O

Example 84 3- (Trifluoromethyl)phenethyl N-{4-[(6,7-dimethoxy-4-quinolyl)oxy]-2,5-dimethylphenyl}carbamate 4-[(6,7-Dimethoxy-4-quinolyl)oxy]-2,5-dimethylaniline (80 mg) was added to toluene/triethylamine = 10/1 (8 ml), and the mixture was heated under reflux to prepare a solution. A solution of triphosgene (125 mg) in methylene chloride was then added to the solution, and the mixture was heated under reflux for 15 min. Subsequently, 3-trifluoromethylphenethyl alcohol (70 mg) was added thereto, and the mixture was further stirredwith heating under reflux for 2 hr. After the completion of the reaction, the reaction solution was allowed to cool to room temperature before distilled water was added thereto. The mixture was subjected to separatory extraction with chloroform, followed by washing with a 1 N aqueous hydrochloric acid solution and saturated brine. The washed solution was dried over sodium sulfate and was concentrated. The residue was purified on a column using chloroform/methanol to give the title compound (79 mg, yield 56%). 1H-NMR (CDCl3, 400 MHz): 8.13 – 8.62 (2H, m), 7.26 – 8.00 (6H, m), 6.96 (1H, s), 6.64 – 6.28 (1H, m), 6.42 (1H, bs), 4.46 (2H, t, J = 6.7 Hz), 4.03 – 4.18 (6H, m), 3.07 – 3.13 (3H, m), 2.23 – 2.30 (3H, m), 2.11 (3H, s) Mass spectrometry value (ESI-MS, m/z): 541 (M++1)

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, 455-01-6, 2-(3-(Trifluoromethyl)phenyl)ethanol.

Reference:
Patent; KIRIN BEER KABUSHIKI KAISHA; EP1243582; (2002); A1;,
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Application of 15833-00-8, Adding some certain compound to certain chemical reactions, such as: 15833-00-8, name is 2-(2-Aminophenyl)propan-2-ol,molecular formula is C9H13NO, 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 15833-00-8.

2-(2-aminophenyl)propan-2-ol (1.19 g, 7.87 mmol) was suspend in dioxane (10 mL) and added carbonyldiimidazole (1.53 g, 9.44 mmol) and stirred for 2 h at room temperature. Aqueous HCl (I N, 15 mL) was added and the reaction was extracted with ethyl acetate (3×20 mL). The combined organic layers were washed with IN HCl and brine, dried and concentrated to give 4,4-dimethyl-lH-3,l-benzoxazin-2-one as a pale solid (1.34 g, 7.56 mmol, 96%). The product was used as such without further purification in the next step LCMS: 0.70 min; ES+ 178 ( M+H+); lH NMR (CHLOROFORM-d, 400MHz): delta (ppm) 9.08 (br s, 1H), 7.24 (t, 1H), 7.14 (d, 1H), 7.07 (t, 1H), 6.89 (d, 1H), 1.73 (s, Step 3: 6-bromo-4.4-dimethyl-lH-3.1-benzoxazin-2-one

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. 15833-00-8, 2-(2-Aminophenyl)propan-2-ol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; THE REGENTS OF THE UNIVERSITY OF CALIFORNIA; SYNGENTA PARTICIPATIONS AG; CUTLER, Sean, R.; LACHIA, Mathilde, Denise; WENDEBORN, Sebastian, Volker; GODFREY, Christopher, Richard Ayles; SABBADIN, Davide; (82 pag.)WO2018/17490; (2018); A1;,
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