Category: alcohols-buliding-blocks

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 2425-41-4, name is (2-Phenyl-1,3-dioxane-5,5-diyl)dimethanol. This compound has unique chemical properties. The synthetic route is as follows. Application In Synthesis of (2-Phenyl-1,3-dioxane-5,5-diyl)dimethanol

(8) A mixture of 2-phenyl-5,5-dihydroxymethyl-1,3-dioxane (2.2 g, 0.01 mol)4-nitrophthalonitrile (1.73 g, O. Olmol),Potassium carbonate (6.9 g, 0.05 mol)Add N, N-dimethylformamide, 50 mL; (9) The reaction was heated at 80 C for 12 hours;(10) After the reaction was stopped, the potassium carbonate was filtered off, the solvent was removed,Column chromatography using methanol / dichloromethane = 1/200 phase gave a white solid which was recrystallized from n-hexane / methylene chloride in a yield of 42%

With the rapid development of chemical substances, we look forward to future research findings about 2425-41-4.

Reference:
Patent; Shandong University , Weihai; BAI, MING; LU, RAN; WAN, PEIHONG; (8 pag.)CN104557949; (2016); B;,
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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. 78573-45-2, name is 3-(3-(Trifluoromethyl)phenyl)propan-1-ol, molecular formula is C10H11F3O, 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 3-(3-(Trifluoromethyl)phenyl)propan-1-ol

2.51 g (14.7 mmol) of (R)-1-(1-naphthyl)-ethylamine and 3.01 g (14.7 mmol) of 3-[3-(trifluoromethyl)phenyljpropanol are weight into a flask. The mixture is diluted with 6 ml of toluene and 53 mg (0.45 mol percent) of {IrCp*Cl2]2 is added. The mixture is heated in a bath at t=110 °C under a reflux condenser in the nitrogen atmosphere for 20 hours. After cooling down, the reaction mixture is diluted with a mixture of hexane and ethyl acetate. On addition of a solution of hydrogen chloride in diethylether, a solid salt is formed and by sucking it off 4.83 g (83 percent) of Cinacalcet hydrochloride is obtained in a purity of 97.8 percent (HPLC). The method described in Example 1 was used for HPLC determination.

With the rapid development of chemical substances, we look forward to future research findings about 78573-45-2.

Reference:
Patent; ZENTIVA, K.S.; VLASAKOVA Ruzena; HAJICEK Josef; WO2013/75679; (2013); A1;,
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Electric Literature of 5343-92-0, 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 5343-92-0, name is 1,2-Pentanediol. This compound has unique chemical properties. The synthetic route is as follows.

IFO therefore was electrochemically oxidized in acetonitrile in the presence of various alcohols with 5 carbon atoms. The reaction was stopped when all the starting material appeared to be consumed as monitored by TLC. At the end of the reaction, sodium bicarbonate (1 Eq.) was added to the medium to neutralize electrogenerated hydrons. The proportions of the various diastereomers were determined on the crude reaction mixture by 31P-NMR before being isolated by ?flash chromatography?.

According to the analysis of related databases, 5343-92-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; INSTITUT GUSTAVE ROUSSY; Paci, Angelo; Martens, Thierry; Rivard, Michael; Couvreur, Patrick; Desmael, Didier; Caron, Joachim; US2013/261088; (2013); 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. 14320-38-8, name is Cyclopent-3-enol, molecular formula is C5H8O, 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. Recommanded Product: Cyclopent-3-enol

To a dry, argon purged three-neck round bottom flask (1000 mL) were added anhydrous dichloromethane (100 mL) and Et2Zn (28 mL, 273 mmol) at 0 C. (CAUTION: Source of argon can not be from needle. Use appropriate glass adapter only. A second bubbler can also be attached to the flask to prevent excessive pressure build up.) Cyclopenten-3-ol (10.0 mL, 119 mmol) was then added dropwise (large quantity of ethane gas was produced) to the flask and the reaction mixture was allowed to stir until the evolution of gas had ceased. Diiodomethane (22 mL, 242 mmol) was then added dropwise over a period of 30 minutes. The reaction was allowed to warm to room temperature and continued to stir overnight under a positive flow of argon, at which point TLC analysis had indicated complete disappearance of the starting alcohol. The reaction was then diluted with CH2Cl2 and quenched with 2M HCl (white precipitate should be completely dissolved). The biphasic mixture was poured into a reparatory funnel and the organic layer was collected. The solvent was removed under reduced pressure until 100 mL of material containing compound 301 remained.

With the rapid development of chemical substances, we look forward to future research findings about 14320-38-8.

Reference:
Patent; GILEAD SCIENCES, INC.; Delaney, William E.; Link, John O.; Mo, Hongmei; Oldach, David W.; Ray, Adrian S.; Watkins, William J.; Yang, Cheng Yong; Zhong, Weidong; US2013/273005; (2013); A1;,
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Adding a certain compound to certain chemical reactions, such as: 346-06-5, (2-(Trifluoromethyl)phenyl)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, Safety of (2-(Trifluoromethyl)phenyl)methanol, blongs to alcohols-buliding-blocks compound. Safety of (2-(Trifluoromethyl)phenyl)methanol

General procedure: To a soln. or suspension of intermediate A-3 or E-3 (1 eq) and alcohol BB-9 (1.1 to 6 eq) in toluene (3.4 to 24 mL/mmol) was added a 1 M soln. of (tributylphosphoranylidene)acetonitrile in toluene (1.1 to 2 eq) under argon. The rxn mixture was heated to a given temperature and stirred for a given time (see (1477) Table ). When necessary to reach completion of the rxn, extra amounts of a 1M soln. of (tributylphosphoranylidene)acetonitrile in toluene (0.2 eq) were sequentially added under argon. It was quenched with water or a sat. aq. soln. of NaHC( and extracted with EtOAc or DCM. The combined org. phases were washed with brine, dried over MgS04 and concentrated in vacuo. The crude was purified by CC using Hept/EtOAc or DCM/MeOH. When necessary, an additional purification by prep. LC-MS using methods 2, 3, 4 or 5 was performed.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,346-06-5, (2-(Trifluoromethyl)phenyl)methanol, and friends who are interested can also refer to it.

Reference:
Patent; IDORSIA PHARMACEUTICALS LTD; FROIDEVAUX, Sylvie; HUBLER, Francis; MURPHY, Mark; RENNEBERG, Dorte; STAMM, Simon; (266 pag.)WO2019/137927; (2019); 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. 623-04-1, name is (4-Aminophenyl)methanol, molecular formula is C7H9NO, 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. COA of Formula: C7H9NO

PSA targeted prodrug was synthesized via scheme 1. The PSA targeting peptide was synthesized by solid phase peptide synthesis. Commercially available Fmoc-protected leucine was coupled with /j>-aminobenzyl alcohol (PAB) by following standard amide coupling protocol. Following bromination, intermediate 2 was reacted with sodium diethyl dithiocarbamate to give 3. Fmoc deprotection of 3 affords Leu-PAB-DTC 4. Compound 4 was coupled to the PSA targeting peptide synthesized via solid phase peptide synthesis to give PSA-DTC, PSA-targeting prodrug (Scheme 1). A) p-Aminobenzyl alcohol, HBTU, 4% NMM in DMF, 3h, rt, 63%; B) PBr3, Dry THF, 3 h, 0 C, 78%; C)(i) Sodium diethyldithiocarbamate, Dry THF, 12 h, rt (ii) 1% DBU in THF, 5 min, rt, 85%; D) FmocRSSYYS, HOBt, EDC, DIPEA, DMF, 12 h, rt; E) 20% piperidine in DMF, 3 h, rt.

With the rapid development of chemical substances, we look forward to future research findings about 623-04-1.

Reference:
Patent; DUKE UNIVERSITY; FRANZ, Katherine, J.; BAKTHAVATSALAM, Subha; ZHANG, Tian; GEORGE, Daniel; SLEEPER, Mark; (88 pag.)WO2019/10231; (2019); 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. 456-47-3, name is 3-Fluorobenzyl alcohol. A new synthetic method of this compound is introduced below., HPLC of Formula: C7H7FO

2-Bromo-4-nitrophenol (4.86 g, 0.0223 mol), triphenylphosphine (7.6 g, 0.0290 mol), 3-fluorobenzylalcohol (3.65 g, 0.0290 mol) were combined and dissolved in THF (89 mL). The reaction temperature was cooled to 0 C. and DIAD (4.50 g, 0.0290 mol) was added. The reaction was allowed to warm slowly to room temperature and stirred for 3 hours before it was diluted with water (100 mL) and EtOAc (100 mL). The layers were separated and the aqueous layer was extracted with EtOAc (200 mL*2). The organic extracts were combined and washed with brine, followed by drying over sodium sulfate. The volatiles were removed in vacuo and the residual semi-solid was treated with diethyl ether. The solids were removed by filtration. The volatiles from the resulting filtrate were removed in vacuo and the material was purified using EtOAc:Hexanes (90/10) in a biotage LC system to afford the title compound as a yellow solid (3.73 g, 68% yield). 1H NMR (DMSO-d6) delta 8.43 (d, 1H); 8.26 (m, 1H); 7.45 (m, 1H); 7.38 (d, 1H); 7.30 (m, 2H); 7.17 (m, 1H); 5.39 (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, 456-47-3, 3-Fluorobenzyl alcohol.

Reference:
Patent; NOVARTIS AG; Lackey, Karen Elizabeth; Mullin, Robert J.; Spector, Neil; Wood, III, Edgar Raymond; Xia, Wenle; (22 pag.)US2015/366868; (2015); 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.3391-86-4, name is Oct-1-en-3-ol, molecular formula is C8H16O, molecular weight is 128.21, as common compound, the synthetic route is as follows.Safety of Oct-1-en-3-ol

General procedure: Hydration reactions were carried out in Schlenk tube under N2atmosphere. The reaction mixture was prepared dissolving 5 mg(6.5 lmol) of catalyst 2 in 3 mL of H2O. The mixture was degassedand 1.5 mmol of corresponding acetonitrile substrate was addedwith micropipette to stirred solution. The reaction was allowedfor heating at 110 C using oil bath or microwave-assisted heating.The isomerization reactions of allylic alcohols were conductedSchlenk tube under N2 atmosphere. The reaction mixture wasprepared dissolving 3 mg (3.9 lmol) of catalyst 2 in 2 mL ofappropriate solvent (DMF, EtOH or H2O). The mixture wasdegassed and 1 mmol of corresponding allylic alcohol substratewas added with micropipette to stirred solution. The reactionwas allowed for heating using oil bath.The reaction solutions were analyzed by regular sampling usingGC/FID (Hewlett Packard) equipped with Beta DEX 120(30 m 0.25 mm 0.25 lm) 30 m long column. The degrees ofconversion were calculated on the basis of the ratio of areas ofthe substrate material and the products determined from correspondingchromatograms. The optimization of chromatographicmethods and the calibration procedures for detection of productsas well as substrates were realized by injection of authenticcommercial samples.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,3391-86-4, Oct-1-en-3-ol, and friends who are interested can also refer to it.

Reference:
Article; Dikhtiarenko, Alla; Khainakov, Sergei; Garcia, Jose R.; Gimeno, Jose; Inorganica Chimica Acta; vol. 454; (2017); p. 107 – 116;,
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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. 2568-33-4, name is 3-Methylbutane-1,3-diol, molecular formula is C5H12O2, 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 3-Methylbutane-1,3-diol

Into a 1 L three-necked flask equipped with a stirrer, a dry air inlet tube, a thermometer, a distillation column (inner diameter 25 mm × height 300 mm, packing tower packed with 6 mm McMahon packing) and a distillation head,100 g of 3-methyl-3-hydroxy-1-butyl alcohol, 5.1 g of Zn-acetylacetonate and 33 g of hexane as a catalyst, and the inside of the system was heated to 100 to 110 C. with stirring. 15 g of hexane was withdrawn from the top of the distillation column.After cooling the inside of the system to 40 C., 240 g of methyl methacrylate and 0.24 g of 2,2,6,6-tetramethyl-4-hydroxypiperidine-N-oxide as a polymerization inhibitor were charged and stirred while blowing in a small amount of air While heating the inside of the system to 100 to 130 C. Methanol produced as the reaction proceeds proceeds by azeotropic distillation with methyl methacrylate,The reaction was gradually withdrawn from the top of the distillation column to proceed the reaction.The conversion rate of 3-methyl-3-hydroxy-1-butyl alcohol after 7 hours from the start of the reaction was 97.5%3-methyl-3-hydroxy-1-butyl alcoholThe yield of 3-methyl-3-hydroxy-1-butyl methacrylate was 77.0%, and the diester yield based on 3-methyl-3-hydroxy-1-butyl alcohol was 10.8%

With the rapid development of chemical substances, we look forward to future research findings about 2568-33-4.

Reference:
Patent; Mitsubishi Gas Chemical Company; Kushida, Eriko; Takemoto, Makiko; (16 pag.)JP2018/135285; (2018); A;,
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Reference of 929-06-6, 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 929-06-6, name is 2-(2-Aminoethoxy)ethanol. This compound has unique chemical properties. The synthetic route is as follows.

compound C (10.0 g, 0.095 mol) was dissolved in 50 mL of methylene chloride and triethylamine (11.55 g, 0.114 mol) was added to it. The solution was cooled in an ice-bath and di-tert-butylcarbonate (22.83 g, 0.105 mol) in 30 mL of methylene chloride was added through an additional funnel. The reaction was slowly warmed up to room temperature and stirred at room temperature overnight. The reaction was extracted with water and the organic phase was washed with diluted HCl solution and dried over magnesium sulfate. Solvent was evaporated and the crude product was purified by column to give 12.43 g of pure product as an oil, 64% yield. 1H NMR (CDCl3) delta (ppm): 1.45 (s, 9 H), 3.30-3.35 (m, 2 H), 3.48-3.59 (m, 4 H), 3.71-3.76 (m, 2 H), 5.47 (s, br, 1 H).

According to the analysis of related databases, 929-06-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Zheng, Shiying; Wang, Ruizheng; Che, Wenyi; US2008/95699; (2008); A1;,
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