Month: July 2021

Application of 13330-96-6, 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. 13330-96-6, name is 4-(Dimethylamino)butan-1-ol, molecular formula is C6H15NO, 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.

Tetramethylazodicarboxamide (0.4 mmol) was added to an ice-cooled solution of phenol (24, 0.2 mmol), alcohol (0.3 mmol) and tributylphosphine (0.4 mmol) in anhydrous benzene (1 mL). The reaction mixture was then heated at 90 C for 12 hours. The reaction mixture was concentrated and the residue was purified by column chromatography (SiO2, Methanol: DCM, 2:98) to afford a white amorphous solid (56%). The product was dissolved in MeOH/THF (1:1) and palladium on carbon (10% w/w, 20 mg) was added to the solution under inert atmosphere. The resulting mixture was then stirred under hydrogen atmosphere overnight. The reaction mixture was filtrated through celite and concentrated to get phenol (~100%). Diisopropylazodicarboxylate (0.2 mmol) was added to an ice-cooled solution of phenol (0.1 mmol), N-methyl-4-hydroxy-piperidine (0.15 mmol) and triphenylphosphine (0.2 mmol) in anhydrous THF (1 mL) and resulting solution was then allowed to stir at room temperature for 12 hours. The reaction mixture was concentrated under reduced pressure and the residue was purified by prep-TLC (SiO2, Methanol:DCM:NH4OH, 1:10:0.1) to afford a white amorphous solid (30%).

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 13330-96-6, 4-(Dimethylamino)butan-1-ol.

Reference:
Article; Garg, Gaurav; Zhao, Huiping; Blagg, Brian S.J.; Bioorganic and Medicinal Chemistry; vol. 25; 2; (2017); p. S1 – S58;,
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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. 4415-73-0, name is 1,1-Cyclobutanedimethanol, the common compound, a new synthetic route is introduced below. Formula: C6H12O2

B. Preparation of cis-1, 2-bis-(bromomethyl) cyclobutane (XXI) To 44 g of phosphorous tribromide (-10 C.) was added dropwise 10.7 g of distilled XX over a 1 hour period. The reaction mixture was warmed to 25 C. and stirred for 2 hours, then heated to 80-85 C. for 18 hours. The reaction mixture was cooled in ice and cold water added. The layers were separated and the aqueous layer was extracted with methylene chloride. The organic extracts were combined, washed with 5% aqueous sodium carbonate and water, then distilled to yield 13.8 g of the title compound XXI as a purple oil, bp 86 (vacuum pump): ir (CHCl3) 3.4, 7.0-8.1mu (no OH signal observed); nmr delta 1.3-2.5 (m, 4), 2.8 (m, 2), and 3.5 (m, 2).

The synthetic route of 4415-73-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Miles Laboratories, Inc.; US4206127; (1980); A;,
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Application of 3279-95-6, Adding some certain compound to certain chemical reactions, such as: 3279-95-6, name is 2-(Aminooxy)ethanol,molecular formula is C2H7NO2, 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 3279-95-6.

EXAMPLE 802-(2-Fluoro-4-iodophenylamino)-5,5-dimethyl-8-oxo-5,6J,8-tetrahydro-4H-thieno[2,3- clazepme-S-carboxylic acid (2-hvdroxyethoxy)amide; Example 2 (1.0 g, 2.6 mmol), EDC (362 mg, 2.9 mmol), etaOBT (300 mg, 2.9 mmol), NMM (427 mg, 5.2 mmol) and 0-(2-hydroxyethyl)hydroxylamine (163 mg, 2.6 mmol) in DMF (10 mL) and DCM (9 mL) were stirred for 48 h. The reaction mixture was poured onto water and extracted with DCM, the unreacted acid removed by filtration and the remaining organic phase washed with IM aqueous HCl then dried over sodium sulphate and concentrated in vacuo. Chromatography (silica; ethyl acetate) yielded the title compound. deltaeta (DMSOd6) 11.22 (IH, br s), 8.82 (IH, br s), 7.93 (IH, t, J4.6 Hz), 7.64 (IH, dd, J 10.7, 2.1 Hz), 7.48 (IH, d, J 8.5 Hz), 7.08 (IH, t, J 8.5 Hz), 4.71 (IH, br s), 3.81-3.74 (2H, m), 3.59-3.50 (2H, m), 2.86 (2H, d, J5.0 Hz), 2.65 (2H, s), 0.97 (6H, s). LCMS (ES+) RT 2.85 minutes, 534 (M+H)+.

According to the analysis of related databases, 3279-95-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; UCB PHARMA S.A.; WO2008/20206; (2008); A2;,
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Adding a certain compound to certain chemical reactions, such as: 83647-43-2, (3-Bromo-2-methylphenyl)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, 83647-43-2, blongs to alcohols-buliding-blocks compound. HPLC of Formula: C8H9BrO

To a solution of (3-bromo-2-methyl-phenyl)-methanol (2 g, 9.9 mmol) in DCM (25 mL) is added phosphorous tribromide (1.76 mL, 14.9 mmol) at 0 C and the reaction mixture is allowed to warm to room temperature and stuffed 1 hour. The reaction mixture is diluted with DCM (20 mL), quenched with aqueous NaHCO3 solution, andextracted with DCM (3×50 mL). The combined organic extracts are washed with water (10 mL) and brine (10 mL), dried over anhydrous Na2504, filtered, and evaporated to dryness to give the title compound (2 g,77%). LC-MS m/z 264 [M+H]+.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,83647-43-2, its application will become more common.

Reference:
Patent; ELI LILLY AND COMPANY; HAMDOUCHI, Chafiq; MAITI, Pranab; MILLER, Anne Reifel; WO2015/105779; (2015); A1;,
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Synthetic Route of 6966-10-5, 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. 6966-10-5, name is (3,4-Dimethylphenyl)methanol. A new synthetic method of this compound is introduced below.

General procedure: General procedure for the synthesis of phenanthridines 3: To a 25 mL tube containing a magnetic stir bar, was added 2-isocyanobiphenl 1 (0.2mmol, 1.0 equiv), Fe(acac)2 (20% mmol, 25.4mg), 4 AMS (100mg), TBHP (5.5M in nonane, 0.15ml, 0.8mmol, 4.0 equiv), benzyl alcohol 2 (0.8mmol, 4.0 equiv), and MeCN (2ml). The resulting mixture was heated under O2 at 100C for 24h. The solvent was removed under vacuum, and the residue was purified by column chromatography (SiO2, petroleum ether/ethyl acetate=1:10) to provide the desired products 3.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,6966-10-5, (3,4-Dimethylphenyl)methanol, and friends who are interested can also refer to it.

Reference:
Article; Nie, Ziyi; Ding, Qiuping; Peng, Yiyuan; Tetrahedron; vol. 72; 50; (2016); p. 8350 – 8357;,
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Adding a certain compound to certain chemical reactions, such as: 1074-61-9, (4-Vinylphenyl)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, Recommanded Product: 1074-61-9, blongs to alcohols-buliding-blocks compound. Recommanded Product: 1074-61-9

Using a reaction scheme adapted from literature [32] , phosphorous tribromide (18.4 g, 6.4 mL, 68 mmol) dissolved in diethyl ether (10 mL) was added to alcohol 1 (5.9 g, 44.3 mmol) in Et2O (500 mL) at 0 C under N2. After 1 h, additional phosphorous tribromide (18.4 g, 6.4 mL, 68 mmol) was added. The reaction mixture was stirred for 1 h at room temperature and subsequently cooled to 0 C. Water (100 mL) was slowly added. The solution was extracted with Et2O, and the Et2O layer was washed with saturated NaHCO3, brine and dried over MgSO4. The crude product was purified by silica gel column chromatography using a hexane:EtOAc, (70:30) elutant system to obtain product vinyl benzyl bromide 2. 1H NMR (CDCl3, 500 MHz) delta: 4.48 (s, 2H), 5.26 (dd, J = 11.0, 1.0 Hz, 1H) 5.76 (dd, J = 17.6, 1.0 Hz, 1H) 6.69-6.75 (dd, J = 17.6, 11.0 Hz, 1H), 7.32 (d, J = 8.0 Hz, 2H) 7.41 (d, J = 8.0 Hz, 2H). UV-Vis [chloroform, lambdamax(epsilon)]: 215 nm, 260 nm.

The synthetic route of 1074-61-9 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Balami, Uddhav; Taylor, Darlene K.; Reactive and functional polymers; vol. 81; 1; (2014); p. 54 – 60;,
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Related Products of 3279-95-6, 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 3279-95-6, name is 2-(Aminooxy)ethanol. This compound has unique chemical properties. The synthetic route is as follows.

General procedure: To a solution of 10 mg (0.012 mmol) of compounds 9a or 9b in anhydrous and deoxygenated THF, 2-(aminooxy)ethanol (1.5 mg, 0.02 mmol) and PTSA (2 mg) were added. The reaction was performed in a glass pressure tube (Ace pressure tube from Aldrich), purged with argon and stirred at room temperature for 6 h. The consumption of starting material 9a-b was monitored by TLC and UVeVis spectroscopy. The solvent was removed under reduced pressure when no starting material was detected. The purification was carried out by flash column chromatography in silica gel using dichloromethane:methanol 99:1 as eluent, and the chlorin derivatives were crystallized from CH2Cl2/hexane. 21,22[N,N-dicarbonyl-N-4-(O-2-hydroxyethyloxime)phenyl]-13,17-bis[2-(methoxycarbonyl)ethyl]-2,7,12,18-tetramethyl-18-vinyl-2,21,22,23-tetrahydrobenzo[b]porphyrin (10a): Yield: 7.5 mg; 8.0 mmol; 70%. 1H NMR (CDCl3, 400 MHz) delta (ppm): -2.47–2.39 (sl, 2H); 2.09 (s, 3H); 3.16 (t, 2H, J=7.9 Hz); 3.21 (t, 2H, J=8.1 Hz); 3.41 (s, 3H); 3.46-3.48 (m, 2H); 3.50 (s, 3H); 3.56 (s, 3H); 3.65 and 3.68 (2s, 3H and 3H); 3.73 (t, 2H, J=4.4 Hz); 3.93-3.97 (m, 1H); 4.09-4.07 (m, 2H); 4.18 (t, 2H, J=7.8 Hz); 4.31 (t, 2H, J=7.5 Hz), 4.68 (d, 1H, J=8.7 Hz); 4.72 (br.s,1H); 6.15 (dd, 1H, J=1.3 Hz and 11.5 Hz, H-8(2a)); 6.35 (dd, H, J=1.3 Hz and 17.9 Hz); 6.77-6.74 (m, 2H); 7.17-7.15 (m, 2H); 7.42 (t, 1H, J=5.3 Hz); 7.76 (s, 1H); 8.19 (dd, 1H, J=17.9 and 11.5 Hz); 9.09 (s, 1H, H-20); 9.33 (s, 1H, H-5); 9.68 (s, 1H); 9.86 (s, 1H). 13C NMR (CDCl3,100 MHz) delta (ppm): 11.4 (1CH3); 11.6 (1CH3); 12.3 (1CH3); 21.5 (1CH2); 21.9 (1CH2); 25.6 (1CH2); 26.4 (1CH3);36.6 (1CH2); 37.0 (1CH2); 38.5 (1CH); 50.1 (1CH); 51.7 (1CH3); 51.8(1CH3); 52.3 (1C); 62.0 (1CH2); 75.1 (1CH2); 90.4 (1CH); 93.2 (1CH); 98.0 (1CH); 99.8 (1CH); 115.5 (1CH); 121.3 (1CH2); 126.2 (2CH); 127.1 (2CH); 129.2 (1C); 129.8 (1CH); 130.9 (1C); 131.5 (1C); 132.57 (1C); 132.64 (1C); 133,8 (1C); 133.9 (1C); 136.3 (1C); 136.5 (1C); 138.3 (1C); 138.4 (1C); 139.7 (1C); 148.1 (1CH); 149,6 (1C); 151.1 (1C); 151.4 (1C); 152.1 (1C); 165.8 (1C); 173.4 (1C); 173.8 (1C); 174.6 (1C); 178.4 (1C). HRMS (ESI-TOF): m/z calculated for [M+] 850.3685; found 850.3684. UV-Vis (CH2Cl2) lambdamax nm (log epsilon) 407 (5.14), 503 (4.00), 540 (4.00), 610 (3.57), 668 (4.50).

According to the analysis of related databases, 3279-95-6, the application of this compound in the production field has become more and more popular.

Reference:
Article; Dos Santos, Fabiane A.B.; Uchoa, Adjaci F.; Baptista, Mauricio S.; Iamamoto, Yassuko; Serra, Osvaldo A.; Brocksom, Timothy J.; De Oliveira, Kleber T.; Dyes and Pigments; vol. 99; 2; (2013); p. 402 – 411;,
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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. 456-47-3, name is 3-Fluorobenzyl alcohol, the common compound, a new synthetic route is introduced below. name: 3-Fluorobenzyl alcohol

General procedure: A solution of benzyl alcohol (1 mmol), SCC (1 mol %), 70% TBHP (1 mmol or 3 mmol),and 4-methylpyridine (1.0 mmol) in H2O (2 mL) was stirred at 60 C (or 80 C) for 10 h (or 15 h).The reaction mixture was quenched with a saturated solution of sodium thiosulfate (5 mL) andextracted using dichloromethane (3 10 mL). The combined organic layers were dried over anhydrous Na2SO4, filtrated, and then the solvent was removed under reduced pressure. The residue was purified by flash column chromatography on silica gel with petroleum ether/ethyl acetate as the eluent to obtain the desired product.

The synthetic route of 456-47-3 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Liu, Shi-juan; Zhang, Miao; Lu, Rong; Li, Xiu-ying; Che, Guang-bo; Molecules; vol. 23; 8; (2018);,
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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. 626-18-6, name is 1,3-Benzenedimethanol. A new synthetic method of this compound is introduced below., SDS of cas: 626-18-6

Complex 2 (8.3 mg, 10 mmol), CsOHH2O (0.84 g, 5 mmol),alcohol (5 mmol) was added to a 25 mL schlenk tube and the solutionwas heated at 150 C (oil bath) for 24 h in an open systemunder argon. After cooling to room temperature, the degassedwater (5 mL)was added and the mixturewas extracted with diethylether (3 10 mL). A sample of ether phasewas subjected to the GCMSanalysis and the residual solution was evaporated, then subjected to the NMR analysis. The aqueous phase was acidifiedwith 6 M HCl and extracted with ethyl acetate (5 20 mL). Thecombined organic phasewaswashed with brine (25 mL), dried overanhydrous Na2SO4, and evaporated under reduced pressure, thepure carboxylic acid was collected and weighed for calculating theyield, which was further characterized by its 1H NMR which isconsist with the standard sample.

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, 626-18-6, 1,3-Benzenedimethanol.

Reference:
Article; Dai, Zengjin; Luo, Qi; Meng, Xianggao; Li, Renjie; Zhang, Jing; Peng, Tianyou; Journal of Organometallic Chemistry; vol. 830; (2017); p. 11 – 18;,
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Electric Literature of 100751-63-1, 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. 100751-63-1, name is 6-Bromo-2-naphthylmethanol, molecular formula is C11H9BrO, 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.

c. 6-Bromo-2-naphthaldehyde To a solution of 6-bromo-2-naphthylmethyl alcohol (6.71 g, 28.3 mmol) in CH2Cl2 (350 mL) was added pyridinium chlorochromate (6.71 g, 31.13 mmol) all at once. The mixture visually went from orange-red to black over 30 minutes and 150 mL of ether was added. The black mixture was passed through a silica gel column and eluted with ether. The solvents were evaporated and the solid was further purified on silica gel (hexane:CH2Cl2 1:1) to give 6.25 g of 6-bromo-2-naphthaldehyde (94%) as a white solid. %). 1H NMR (300 MHz; CDCl3): delta7.65 (dd, J1=2.0 Hz, J2=9.0 Hz, 1 H); 7.84 (t, J=8.0 Hz, 2 H); 7.97 (dd, J1=2.0 Hz, J2=8.0 Hz, 1 H); 8.06 (d, J=2.0 Hz, 1 H); 8.29 (s, 1 H); 10.14 (s, 1 H); 13C NMR (300 MHz; CDCl3): ppm 123.5, 123.9, 128.0, 130.1, 130.5, 130.8, 130.9, 133.9, 134.2, 137.1, 191.6.

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 100751-63-1, 6-Bromo-2-naphthylmethanol.

Reference:
Patent; Pfahl, Magnus; Tachdjian, Catherine; Al-Shamma, Hussien A.; Fanjul, Andrea; Pleynet, David P.M.; Spruce, Lyle W.; Wiemann, Torsten R.; Ibarra, Jason B.; US2002/143182; (2002); A1;,
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