Tag: M.W=200-300

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;,
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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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Reference of 261723-33-5, 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. 261723-33-5, name is (2-Bromo-6-fluorophenyl)methanol, molecular formula is C7H6BrFO, 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.

PREPARATION 8 1-Bromo-3-fluorobenzyl bromide To a solution of 1-bromo-3-fluorobenzyl alcohol (1.61 kg, 7.85 mol) in chloroform (14 L) at 0° C. add pyridine (770 mL, 9.52 mol) in one portion (slight exotherm) and stir at 0° C. for 5 min. Add phosphorus tribromide (900 mL, 9.49) dropwise while maintaining the internal temperature below 20° C. and stir the resulting solution overnight while allowing to warm to room temperature. Cool the reaction to 0° C. and quench slowly with ice water (2 L). Transfer to a 50 L flask, separate the layers and then extract the aqueous layer with chloroform (1 L). Wash the combined organic phases with 5percent sulfuric acid (2 L), saturated aqueous sodium bicarbonate (2 L), brine (2 L), dry over magnesium sulfate, filter, and concentrate to obtain the title compound as a yellow oil (1753 g, 83percent). 1H NMR (CDCl3) delta 7.43 (d, 1H), 7.21 (m, 1H), 7.09 (t, 1H), 4.68 (s, 2H).

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 261723-33-5, (2-Bromo-6-fluorophenyl)methanol.

Reference:
Patent; GAVARDINAS, Konstantinos; Jadhav, Prabhakar Kondaji; US2009/163472; (2009); A1;,
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Synthetic Route of 756520-66-8, 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. 756520-66-8, name is 1-(2,6-Dichloro-3-fluorophenyl)ethanol. A new synthetic method of this compound is introduced below.

Step 2 (±)3-(1-(2,6,-dichloro-3-fluorophenyl)ethoxy)-2-nitropyridine [00161] To a solution of triphenylphosphine (24.29 g, 92.6 mmol) in THF (dry, 160 ml_) was added DIAD (18.23 ml_, 92.6 mmol) dropwise at 0 C under N2. After addition of DIAD, a solution of 1-(2,6-dichloro-3-fluorophenyl)ethanol (13.35 g, 63.86 mmol) and 3-hydroxy-2-nitropyridine (10.29 g, 73.44 mmol) in THF (anhydrous, 160 ml_) was added dropwise. The ice-bath was removed and the reaction mixture was allowed to warm to room temperature and stirred at room temperature for 4 hrs. The reaction mixture was concentrated by evaporator to give a yellow residue. A saturated solution of NH4CI (200 ml_) was added. The aqueous phase was extracted with EtOAc (3^150 mL). The combined organic phase was washed with brine (2*80 mL), dried over anhydrous Na2S04, concentrated by evaporation in vacuo to give a yellow residue which was purified by CombiFlash (220 g silica gel column, Hexane/EtOAc) to afford (±)-3-(1-(2,6,- dichloro-3-fluorophenyl)ethoxy)-2-nitropyridine (21.1 g, 100%) as a white solid. [00162] 1HNMR (300 MHz, CDCI3): delta 8.04 (d, 1 H), 7.37 (m, 1 H), 7.30 (dd, 1 H), 7.21 (d, 1 H), 7.09 (t, 1 H), 6.10 (q, 1 H), 1.85 (d, 3 H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,756520-66-8, 1-(2,6-Dichloro-3-fluorophenyl)ethanol, and friends who are interested can also refer to it.

Reference:
Patent; BETA PHARMA CANADA INC.; WANG, Zhaoyin; LI, Lianhai; WANG, Zhigang; WO2013/13308; (2013); A1;,
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Related Products of 1227159-85-4, 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. 1227159-85-4, name is (1-(4-Bromophenyl)cyclobutyl)methanol, molecular formula is C11H13BrO, 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.

(1-(4-Bromophenyl)cyclobutyl)methanol (260 mg, 1.08 mmol), tert-butyldimethyichiorosilane (0.246 mL, 1.29 mmol) and imidazole (151 mg, 2.16 mmol) combined in dimethylformamide (6 mL) at room temperature for 18 hours. Water (20 mL) added and solution extracted with a 1:1 solution of ethyl acetate-heptane. The extract was washed with brine, dried over magnesium sulfate, filtered and concentrated. Crude purified on silica gel, eluding with a gradient from 0 to 30% ethyl acetate in heptane to give ((1-(4-bromophenyl)cyclobutyl)methoxy)(tert-butyl)dimethylsilane (323 mg, 84%) 1H NMR (400 MHz, CHLOROFORM-d) delta ppm -0.15 (s, 6H) 0.82 (s, 9H) 1.77-1.86 (m, 1H) 1.97-2.08 (m, 1H) 2.20-2.26 (m, 4H) 3.59 (s, 2H) 6.98 (d, 2H) 7.37 (d, 2H)

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 1227159-85-4, (1-(4-Bromophenyl)cyclobutyl)methanol.

Reference:
Patent; pfizer Inc; US2010/197591; (2010); A1;,
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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 145691-59-4, name is (3,5-Dibromophenyl)methanol. This compound has unique chemical properties. The synthetic route is as follows. Recommanded Product: 145691-59-4

Into a 100-mL round-bottom flask, was placed (3,5-dibromophenyl)methanol (2 g, 7.52 mmol, 1.00 eq.), dioxane (40 mL), water(4 mL), 2-ethenyl-4,4,5,5-tetramethyl-l,3,2-dioxaborolane (1.2 g, 7.79 mmol, 1.00 eq.), Pd(PPh3)4 (900 mg, 0.78 mmol, 0.10 eq.), potassium carbonate (3.1 g, 22.43 mmol, 3.00 eq.). The resulting solution was stirred for 1 overnight at 100 C. The solids were filtered out. The resulting mixture was concentrated under vacuum. The resulting solution was diluted with 100 mL of H2O. The resulting solution was extracted with 3×100 mL of ethyl acetate and the organic layers combined and dried over anhydrous sodium sulfate and concentrated under vacuum. The residue was applied onto a silica gel column with dichloromethane. This resulted in 1.1 g (69%) of (3-bromo-5- ethenylphenyl)methanol as yellow oil.

With the rapid development of chemical substances, we look forward to future research findings about 145691-59-4.

Reference:
Patent; PRINCIPIA BIOPHARMA INC.; LOU, Yan; OWENS, Timothy Duncan; BRAMELD, Kenneth Albert; GOLDSTEIN, David Michael; (171 pag.)WO2019/99576; (2019); A1;,
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Adding a certain compound to certain chemical reactions, such as: 171011-37-3, (4-Bromo-1,2-phenylene)dimethanol, 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, Recommanded Product: 171011-37-3, blongs to alcohols-buliding-blocks compound. Recommanded Product: 171011-37-3

(1) In 380 ml of diethyl ether was dissolved 19.0 g of 1-bromo-3,4-di(hydroxymethyl)benezene and to the solution was added 112 g of phosphorus tribromide under ice-cooling, after which the resulting mixture was allowed to stand for 3 days. The reaction mixture was added to 1,000 ml of ice water and the pH was adjusted to 7 with sodium hydrogencarbonate, followed by extraction with 1,000 ml of ethyl acetate. The organic layer thus obtained was washed with a saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate, and then distilled under reduced pressure to remove the solvent, whereby 28.5 g of 1-bromo-3,4-di(bromomethyl)benzene were obtained as colorless crystals.

The synthetic route of 171011-37-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Toyama Chemical Co., Ltd.; US6025370; (2000); A;,
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Related Products of 78573-45-2, Adding some certain compound to certain chemical reactions, such as: 78573-45-2, name is 3-(3-(Trifluoromethyl)phenyl)propan-1-ol,molecular formula is C10H11F3O, 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 78573-45-2.

A solution of (R) -N- [1- (1-naphthyl) ethyl] -2-nitrobenzenesulfonamide in toluene (83 g pure)92 g of triphenylphosphine,72 g of 3- (3-trifluoromethylphenyl) propanol and 125 mL of toluene were added and stirred. Adjust the solution temperature to 50 ° C,DiisopropylazodicarboxylateA diluted solution obtained by adding 330 mL of toluene to 71 g was dropped. After the dripping end50 mL of toluene was added and stirred at 50 ° C. for 1 hour.After completion of the reaction, 133 g of anhydrous magnesium chloride and 42 mL of toluene were added. After stirring at 50 ° C. for 2 hours, the liquid temperature was cooled to 0 ° C.The reaction solution was filtered to remove insolubles, and then washed with 415 mL of toluene cooled to 0° 415 mL of tap water was added to the filtrate and stirred, and the aqueous layer was removed by liquid separation operation. The same operation was repeated twice, and the obtained organic layer was concentrated under reduced pressure at 55 ° C. to 1165 mL,(R) -N- [1- (1-naphthyl) ethyl] -3- [3- (trifluoromethyl) phenyl]Propane-2-nitrobenzenesulfonamide tolueneA solution was obtained (pure yield 127 g, pure yield 100percent, chemical purity 92percent).

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. 78573-45-2, 3-(3-(Trifluoromethyl)phenyl)propan-1-ol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Iwaki Pharmaceutical Co Ltd; Nagasaki, Atsushi; Fukushima, Koichi; (8 pag.)JP2019/14687; (2019); A;,
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Application of 7073-69-0, 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. 7073-69-0, name is 2-(2-Bromophenyl)propan-2-ol. A new synthetic method of this compound is introduced below.

General procedure: A DMF solution (8mL) of the o-substituted aryl iodide (0.36mmol), the o-bromobenzyl alcohol (0.36mmol) and norbornene (34mg, 0.36mmol) was added under nitrogen to a Schlenck-type flask, containing Pd(OAc)2 (4mg, 0.018mmol), the phosphine (0.036mmol), when required, and K2CO3 (124mg, 0.90mmol) or CsOPiv (211mg, 0.90). The reaction mixture was stirred at 105C for 24h. After cooling to room temperature the organic layer was diluted with EtOAc (20mL), washed twice with water (20mL) and dried over Na2SO4. The solvent was removed under reduced pressure and the resulting residue was purified by flash chromatography on silica gel using mixtures of hexane-EtOAc as eluent.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,7073-69-0, its application will become more common.

Reference:
Article; Della Ca, Nicola; Fontana, Marco; Xu, Di; Cremaschi, Mirko; Lucentini, Riccardo; Zhou, Zhi-Ming; Catellani, Marta; Motti, Elena; Tetrahedron; vol. 71; 37; (2015); p. 6389 – 6401;,
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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. 5333-42-6, name is 2-octyldodecan-1-ol, molecular formula is C20H42O, 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. Computed Properties of C20H42O

A 500-mL three-necked flask equipped with magnetic stirrer, septum, and thermometer was filled with argon. Triphenylphosphine (33.4 g, 0.127 mol, 1 equiv.) and 200 mL of anhydrous dichloromethane were placed into the flask. The solution was cooled to 0C, and 6.52 mL (20.34 g, 0.127 mol, 1 equiv.) of bromine was added dropwise so that the temperature of the reaction mix- ture was not higher 5C. After bromine addition was completed, the reaction mixture was stirred for 15 min at 0C, 45.36 mL (38.0 g, 0.127 mol, 1 equiv.) of2-octyl-1-dodecanol was added. The reaction mixture was stirred for 12 h at ambient temperature, concen- trated in a vacuum, the resultant suspension was diluted with 100 mL of petroleum ether, and filtered. The filtrate was passed through a thin layer of silica gel, washed with petroleum ether, and concentrated in a vacuum to give 43.61 g (95%) of viscous oil.1H NMR (400 MHz, CDCl3, delta, ppm): 3.47 (d, J =4.7 Hz, 2H), 1.66-1.54 (m, 1H), 1.45-1.17 (m, 32H),0.91 (t, J = 6.7 Hz, 6H).13C NMR (101 MHz, CDCl3, delta, ppm): 39.7, 39.5,32.5, 31.9, 29.8, 29.6, 29.6, 29.5, 29.3, 29.3, 26.5,22.6, 14.1.

With the rapid development of chemical substances, we look forward to future research findings about 5333-42-6.

Reference:
Article; Keshtov; Osipov; Topchiy; Zotova; Konstantinov; Krayushkin; Kuklin; Khokhlov; Doklady Chemistry; vol. 463; 2; (2015); p. 215 – 220; Dokl. Akad. Nauk; vol. 463; 6; (2015); p. 669 – 674,6;,
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