Tag: M.W=100-200

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. 599-67-7, name is 1,1-Diphenylethanol, the common compound, a new synthetic route is introduced below. Recommanded Product: 599-67-7

acetophenone; 2- methyl tetrahydrofuran solution(including 42.6g acetophenone anhydrous ;2- methyltetrahydrofuran 30mL) Slow drop in at room temperature Example 4 ofPhenyl magnesium bromide Grignard reagent Dropfinish,Temperature rise to80 degrees Celsius reaction 3 Hours TLC Monitoring reactioncompletely, Cooling to 5 DEG C. Add 10% hydrochloric acid to the reaction solution pH=6 ~7, Room temperature continues to react for 1hours get the phenylethanol 2- methyltetrahydrofuran, Added 5.08g Sulfonic acidfunctional ionic liquid catalyst, [DBSDMI]OTf (structural formula II),Water separator device, Temperature rise to refluxdehydration reaction 0.5 hours TLC monitoring reaction is complete,Recovery solvent at atmospheric pressure – methyltetrahydrofuran, vacuum distillationresidue from 106 to 110 DEG /2mmHg fraction was colorless oily Liquid 61.3g, Yield was96%, GC content analysis 99.2%, GC test conditions and examples 1.;

The synthetic route of 599-67-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Zhejiang University of Technology; Shangyu Sunfit Chemical Co., Ltd; CHEN, ZHIWEI; SU, WEIKE; JING, LEI; HUANG, SHENGJIAN; CHEN, JIONGMING; (9 pag.)CN103755516; (2016); B;,
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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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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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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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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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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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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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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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Synthetic Route of 765-04-8, 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.765-04-8, name is Undecane-1,11-diol, molecular formula is C11H24O2, molecular weight is 188.3071, as common compound, the synthetic route is as follows.

In a four-necked flask (volume of 1 L) equipped with stirring blades, a thermometer, a dropping funnel and a condenser tube, 300 mL of tetrahydrofuran, 18.8 g (0.10 mol) of undecane-1,1l-diol and 14.4 mg of p-methoxyphenol were charged and dissolved. Subsequently, 9.96 g (0.05 mol) of 2-(2-isocyanatoethoxy)ethyl methacrylate was weighed in a beaker and 150 mL of tetrahydrofuran was added, followed by sufficient stirring and further liquid transfer to the dropping funnel. The four-necked flask was immersed in an oil bath heated to 75 C., and 2-(2-isocyanatoethoxy)ethyl methacrylate was added dropwise so as not to cause boiling of tetrahydrofuran. After completion of the dropwise addition, the reaction was continued for 24 hours while maintaining the temperature of the oil bath, leading to aging. After completion of the aging, the four-necked flask was removed from the oil bath and the reaction product was returned to room temperature, and then HPLC and FT-IR measurements were performed. In that case, a sample obtained by collecting a very small amount of the reaction product using a pipette and removing a solvent using evaporator was used. Analysis conditions of the HPLC measurement are as follows: a column of ZORBAX-ODS, acetonitrile/distilled water of 7/3, a flow rate of 0.5 mL/min, a multi-scanning UV detector, an RI detector and an MS detector. The FT-IR measurement was performed by an ATR method. As a result of the HPLC measurement, peaks of undecane-1,11-diol and 2-(2-isocyanatoethoxy)ethyl methacrylate as raw materials disappeared, and new peak of 2-(2-((((11-hydroxyundecyl)oxy)carbonyl)amino)ethoxy)ethyl methacrylate (molecular weight of 387.52) was confirmed. As a result of the FT-IR measurement, the disappearance of the isocyanate absorption at 2,280 to 2,250 cm-1 and a decrease in intensity of the hydroxy group absorption at around 3,300 cm-1 were confirmed, and the absorption attributed to a urethane group was newly confirmed at 1,250 cm-1. Subsequently, to a tetrahydrofuran solution containing 28.8 g (74.2 mmol) of the precursor compound synthesized by the above-mentioned operation, 15.2 g (74.2 mmol) of (3-isocyanatopropyl)trimethoxysilane was added dropwise while stirring so as not to cause boiling of tetrahydrofuran. In the same manner as in the first stage, a reaction was performed by immersing in an oil bath heated to 75 C. After completion of the dropwise addition, the reaction was continued for 24 hours, leading to aging. After completion of the aging, HPLC and FT-IR measurements were performed. As a result of the HPLC measurement, peaks of 2-(2-((((11-hydroxyundecyl)oxy)carbonyl)amino)ethoxy)ethyl methacrylate and (3-isocyanatopropyl)trimethoxysilane as raw materials disappeared, and new peak of 3,3-dimethoxy-8,22-dioxo-2,9,21,26-tetraoxa-7,23-diaza-3-silaoctacosan-28-ylmethacrylate (molecular weight of 592.80) was confirmed. As a result of the FT-IR measurement, the disappearance of the hydroxy group absorption at around 3,300 cm-1 was confirmed. The chemical structure of the compound synthesized in the present Synthesis Example is mentioned below.

Statistics shows that 765-04-8 is playing an increasingly important role. we look forward to future research findings about Undecane-1,11-diol.

Reference:
Patent; KABUSHIKI KAISHA SHOFU; FUCHIGAMI, Kiyomi; YAMAMOTO, Kenzo; KITADA, Naoya; SHINNO, Kazuya; US2019/300552; (2019); A1;,
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Synthetic Route of 505-10-2, 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. 505-10-2, name is 3-(Methylthio)propan-1-ol, molecular formula is C4H10OS, 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.

The 3-mesylpropanol used as a starting material was prepared as follows: 3-Chloroperoxybenzoic acid (25 g) was added in portions to a solution of 3-methylthiopropanol (5 ml) in methylene chloride (100 ml) while maintaining the reaction temperature at 25 C. The mixture was stirred at ambient temperature for 1 hour. The mixture was filtered and the filtrate was diluted with an aqueous solution of sodium sulphite (6.5 g) in water (200 ml). The organic layer was separated and evaporated. The white residue was triturated under acetone and the resultant solution was evaporated to give a solid which was dissolved in methylene chloride. Aluminum oxide (90 mesh) was added and the mixture was allowed to stand for 15 minutes. The mixture was filtered and the filtrate was evaporated to give 3-mesylpropanol as a colourless oil (4.46 g); NMR Spectrum: (CDCl3) 1.9-2.1 (br s, 1H), 2.15 (m, 2H), 2.95 (s, 3H), 3.2 (t, 2H), 3.85 (t, 2H).

According to the analysis of related databases, 505-10-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Hennequin, Laurent Francois Andre; Crawley, Graham Charles; McKerrecher, Darren; Ple, Patrick; Poyser, Jeffrey Philip; Lambert, Christine Marie Paul; US2003/225111; (2003); A1;,
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