Tag: M.W=200-300

Reference of 83647-43-2 , The common heterocyclic compound, 83647-43-2, name is (3-Bromo-2-methylphenyl)methanol, molecular formula is C8H9BrO, 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 flask charged with (3-bromo-2-methylphenyl)methanol (6.0 g, 30 mmol) was added a 1M trifluoroacetic acid solution of thallium trifluoroacetate (16.2 g, 29.8 mmol). The mixture was stirred at room temperature overnight. The solvent was removed under vacuum, and the residue was pumped under high vacuum for 30 minutes to ensure complete removal of TFA. To the residue was then added palladium(II) chloride (529 mg, 2.98 mmol), lithium chloride (2.53 g, 59.7 mmol), magnesium oxide (2.41 g, 59.7 mmol), and methanol (150 mL). The reaction was flushed with CO twice, and kept under CO at room temperature. Analysis by LC showed a big product spot within 2 hours. To this solution was added ethyl acetate to precipitate the salts. The black solution was filtered through a Celite diatomaceous earth pad, washed with EtOAc, adsorbed onto silica and purified by silica gel chromatography to afford 5-bromo-4-methyl-2- benzofuran-1 (3H)-one. -N R (500 MHz, CDC13) delta ppm 7.71 (d, J= 8.0 Hz, 1H), 7.58 (d, J= 8.0 Hz, 1H), 5.25 (s, 2H), 2,37 (s, 3H).

The synthetic route of 83647-43-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; MERCK SHARP & DOHME CORP.; WALSH, Shawn, P.; PASTERNAK, Alexander; SHI, Zhi-Cai; CATO, Brian; KIM, Esther, Y.; WO2013/66718; (2013); A2;,
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Reference of 78573-45-2 ,Some common heterocyclic compound, 78573-45-2, molecular formula is C10H11F3O, 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.

At room temperature, 15 ml of CHCl,3g 3- (3-trifluoromethylphenyl) propanol was added to a 100 ml reaction flaskA, 2.2 g of triethylamine, stirred and dissolved, and dropwise 2 g of methanesulfonyl chloride. After completion of the dropwise addition, the reaction was carried out for 2 to 3 hours The reaction kettle by adding 9ml 1mol / l of dilute hydrochloric acid stirring, liquid separation. Add 9ml 5% NaHCO3 solution to wash the organic phase, stir Mix and disperse. The organic phase was washed with 9 ml of 25% NaCl, stirred and partitioned. Add anhydrous Na2SO4 to dry and filter. stress reliever The product was distilled to give 5.5 g of a pale yellow liquid in 100% yield.

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; Shanghai Qing Song Pharmaceutical Co., Ltd.; Zhang, Jian; Chen, Xiaona; Zhang, Shubin; Gao, Junfeng; Tan, Zhouhong; (7 pag.)CN106543008; (2017); A;,
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Reference of 2043-47-2, Adding some certain compound to certain chemical reactions, such as: 2043-47-2, name is 1H,1H,2H,2H-Nonafluoro-1-hexanol,molecular formula is C6H5F9O, 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 2043-47-2.

Comparative Example 1In a 100-ml, three-necked glass reactor were placed 50 ml of methylene chloride, 10 g (38 mmol) of 3,3,4,4,5,5,6,6,6-nonafluorohexanol, 10 g (139 mmol) of acrylic acid, 0.1 g of a polymerization inhibitor, Sumilizer GM and 0.2 of toluenesulfonic acid. The mixture was heated. A reaction was allowed to proceed while distillation was made under normal pressure to remove the generated water together with methylene chloride. Every time when the amount of methylene chloride became small and the reactor-inside temperature exceeded 43 C., fresh methylene chloride was added into the reactor, to conduct the reaction for total 10 hours. At this point, the conversion was 82% and the selectivity was 84%.

According to the analysis of related databases, 2043-47-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; TOKUYAMA CORPORATION; DAIKIN INDUSTRIES, LTD.; US2009/23948; (2009); A1;,
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Application of 17100-58-2, 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 17100-58-2, name is (4-Bromo-2-methylphenyl)methanol. This compound has unique chemical properties. The synthetic route is as follows.

4-bromo-2-methyl-l-(phenoxymethyl) benzene. To a solution of (4-bromo-2- methylphenyl)methanol (1 g, 5 mmol), phenol (525 mg, 5.6 mmol) and triphenylphosphine (2.2 g, 8.4 mmol) in tetrahydrofuran (30 mL) was added diisopropyl azodicarboxylate (1.7 g, 8.4 mmol) at 0C. The mixture was stirred at 20C for 12 hours. Water (15 mL) was added to the mixture and then extracted with ethyl acetate (35 mL x 3). The combined organic phase was dried by sodium sulfate, and then filtered. The filtrate was concentrated in vacuo and the residue was purified by column chromatography (silica gel, petroleum ether/ethyl acetate = 5:1) to give 4-bromo-2-methyl-l-(phenoxymethyl) benzene (640 mg, 46%).

According to the analysis of related databases, 17100-58-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; CONSTELLATION PHARMACEUTICALS; ALBRECHT, Brian, K.; AUDIA, James, Edmund; COOK, Andrew; GAGNON, Alexandre; HARMANGE, Jean-christophe; NAVESCHUK, Christopher, G.; WO2013/75083; (2013); A1;,
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Electric Literature of 486460-26-8, 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 486460-26-8, name is (4-Bromo-2,5-difluorophenyl)methanol. This compound has unique chemical properties. The synthetic route is as follows.

To a solution of 2 g (8.44 mmol) of 4-bromo-2,5-difluorobenzoic acid (prepared according to the procedure of Ishikawa et al., Kogyo Kagaku Zasshi, pg 972-979, 1970) in 20 mL of tetrahydrofuran was added 40 mL of a 1M solution of borane-tetrahydrofuran complex. The solution was heated under reflux for 64 h, cooled to ambient temperature and 100 mL of methanol was added. The reaction was then heated for a further 2 h, cooled and concentrated in vacuo. Purification by flash chromatography (silica gel, 9:1 hexane:ethyl acetate) afforded 1.6 g of 4-bromo-2,5-difluorobenzyl alcohol. To a solution of 1.3 g (5.6 mmol) of 4-bromo-2,5-difluorobenzyl alcohol in 20 mL of dichloromethane at 0 C. was added 2.27 g (6.7 mmol) of carbon tetrabromide and 1.8 g (6.7 mmol) of triphenylphosphine. The reaction was stirred for 2 h at this temperature, the solvent was removed in vacuo and the residue stirred with 100 mL of diethyl ether. The solution was filtered, concentrated in vacuo, and purified by flash chromatography (silica gel, 9:1 hexane:ethyl acetate) to afford 1.5 g of the title compound.

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 486460-26-8, (4-Bromo-2,5-difluorophenyl)methanol.

Reference:
Patent; Merck Sharp & Dohme Corp.; Edmondson, Scott D.; Fisher, Michael H.; Kim, Dooseop; Maccoss, Malcolm; Parmee, Emma R.; Weber, Ann E.; Xu, Jinyou; US2015/359793; (2015); 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. 24034-73-9, name is (2E,6E,10E)-3,7,11,15-Tetramethylhexadeca-2,6,10,14-tetraen-1-ol, molecular formula is C20H34O, 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. SDS of cas: 24034-73-9

A dry reaction flask equipped with a stir bar and N2 inlet was charged with geranylgeranyl alcohol 9 (0.087 g, 0.3 mmol), pyridine (0.048 mL, 0.6 mmol) in DCM (2 mL). To it was added, methanesulfonyl chloride 25a (0.035 mL, 0.45 mmol) and stirred for 48 h at room temperature. The reaction was followed by TLC. After the completion of the reaction, it was quenched with water (10 mL), extracted with DCM (3*20 mL) and the combined DCM solution was washed with 2N NaOH solution (20 mL) followed by water (20 mL). The DCM layer upon drying over anhydrous Na2SO4 was evaporated and the residue was purified by silica gel column chromatography using n-hexanes the 1-2% EtOAc in n-hexanes to afford the desired sulfonate 26a. Yield: 0.066 g (66%); TLC Rf: 0.54 (10% EtOAc/n-Hexanes); LCMS: MS (m/z): 367.10 (M-H).

With the rapid development of chemical substances, we look forward to future research findings about 24034-73-9.

Reference:
Patent; Coyote Pharmaceuticals, Inc.; Serizawa, Hiroaki; Argade, Ankush B.; Datwani, Akash; Spencer, Natalie; US2013/85283; (2013); A1;,
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Related Products of 32328-03-3, 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 32328-03-3, name is Diethyl 3-hydroxyglutarate. This compound has unique chemical properties. The synthetic route is as follows.

A 3-Methoxypentane-1,5-diol 25 ml of methyl trifluoromethylsulfonate are added to a solution of 30 g of diethyl 3-hydroxyglutarate and 33 ml of 2,6-di-tert-butylpyridine in 500 ml of DCM and the mixture is refluxed for 5 hours. After cooling, 500 ml of a 0.5N solution of HCl are added, the organic phase is decanted and dried over magnesium sulfate and the solvent is evaporated off under vacuum. The solid obtained is taken up with 200 ml of anhydrous THF, the mixture is filtered and the filtrate is then cooled to -5 C. 160 ml of a 1M solution of lithium aluminum hydride in THF are then added slowly and the mixture is stirred for 16 hours, the temperature being allowed to rise to RT. The reaction mixture is cooled to 0 C. and 5.5 ml of water, 18 ml of a 15% solution of NaOH and 5.5 ml of water are added successively. The mineral salts are filtered off and the filtrate is evaporated under vacuum to give the expected product after distillation under reduced pressure. B.p.=104 C. under 1.5 Pa.

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 32328-03-3, Diethyl 3-hydroxyglutarate.

Reference:
Patent; Sanofi; US5618833; (1997); A;,
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Related Products of 355-80-6, 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.355-80-6, name is 2,2,3,3,4,4,5,5-Octafluoro-1-pentanol, molecular formula is C5H4F8O, molecular weight is 232.0719, as common compound, the synthetic route is as follows.

To a dispersion prepared of 11.22 g (0.2 mol) of KOH and 100 mL of acetonitrile, a portion of 46.4 g (0.2 mol) of 1,1,2,2,3,3,4,4-octafluoropentan-5-ol was added and the mixture was stirred at r.t. for 1.5 h, then 0.22 mol of allyl chloride was added. Then mixture was refluxed for 5 h and kept at r.t. for 24 h. The precipitate was separated by filtration and was washed with cold acetonitrile. The solvent was removed by rotary evaporation and obtained product was purified by trap to trap distillation to give colorless liquid yield 89%. H NMR (CDCl3, delta, ppm): 6.96 (m, 1H, CHF2), 5.79 (m, 1H, CH=CH2), 5.19 (t, 2H, CH2=CH-), 4.04 (d, 2H, CH2O), 3.81 (t, 2H, OCH2CF2),13C NMR (CDCl3, delta, ppm): 133.09 (CH=CH2), 118.98 (CH2=CH), 115.66 (CF2), 111.13 (CF2H), 107.77 (CF2), 104.40 (CF2), 73.55 (CH2O), 66.42 (OCH2). MS (EI, m/z): 273.3 (10.1), 272.2 (91.0) [M+], 95.0 (14.6), 84.0 (9.3), 71.1 (100), 69.1 (26.1), 57.1 (23.3), 56.1 (9.4), 51.0 (31.7).

Statistics shows that 355-80-6 is playing an increasingly important role. we look forward to future research findings about 2,2,3,3,4,4,5,5-Octafluoro-1-pentanol.

Reference:
Article; Januszewski, Rafa?; Kownacki, Ireneusz; Maciejewski, Hieronim; Marciniec, Bogdan; Journal of Organometallic Chemistry; vol. 846; (2017); p. 263 – 268;,
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Reference of 7073-69-0 ,Some common heterocyclic compound, 7073-69-0, molecular formula is C9H11BrO, 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.

C. 3,3-dimethyl-3H-benzo[c][1,2]oxaborol-1-ol To a solution of 2-(2-bromo-phenyl)-propan-2-ol (4.0 g, 18.6 mmol, prepared as described in Egan, W. et al. J. Am. Chem. Soc., 1971, 93, 6205) in 60 mL of anhydrous THF under argon at -78 C. was slowly added n-butyl lithium (15 mL, 2.5 M). The mixture was stirred at -78 C. for 2 h, and then triisopropylborate (5.5 mL, 24.2 mmol) was added to the mixture. The mixture was allowed to warm to room temperature and stirred at room temperature for 12 h. The mixture was then cooled to 0 C. and hydrochloric acid (10 mL, 1N) was added to the mixture until pH was <5. The mixture was then stirred at room temperature for 1 h. The two layers were separated. The aqueous layer was extracted twice with ethyl acetate. The organic layers were combined, dried with anhydrous sodium sulfate and filtered. The filtrate was concentrated under reduced pressure to afford a yellow oil. The oil was purified by chromatography (silica, EtOAc: hexanes,1:3) to afford a white solid (1.16 g, 40%). 1H NMR (400 MHz, CDCl3) delta (ppm): 7.53 (m, 1H), 7.36 (m, 2H), 7.28 (m, 1H), 1.62 (s, 3H), 1.61 (s, 3H). 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. 7073-69-0, 2-(2-Bromophenyl)propan-2-ol, other downstream synthetic routes, hurry up and to see. Reference:
Patent; Cheung, Wing S.; Parks, Daniel J.; Parsons, William H.; Patel, Sharmila; Player, Mark R.; US2008/146637; (2008); A1;,
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Application of 17100-58-2, 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 17100-58-2, name is (4-Bromo-2-methylphenyl)methanol. This compound has unique chemical properties. The synthetic route is as follows.

Description 10: [2-methyl-4-(4,4,5,5-tetramethyl-1 ,3,2-dioxaborolan-2- yl)phenyl]methanol (D10); 4-bromo-2-methyl-benzyl alcohol (D8f, 3Og, 150 mmol), bis(pinacolato)diboron (40 g, 156 mmol), Pd(dppf)CI2(ll) (8 g, 10 mmol), and potassium acetate (44 g, 448 mmol) were dissolved in 1 ,4-dioxane (600 ml_), and the reaction mixture was heated to reflux under N2 for 4 h. After cooling, the reaction mixture was filtered, and the filtrate was concentrated. Purification by column chromatography (silica gel; petroleum ether: ethyl acetate = 5:1 ) afforded the title compound as a red oil (34 g, yield: 90%). 1H NMR (400 MHz, DMSO-c/6) J7.50-7.38 (m, 3H), 5.14 (t, 1 H), 4.51 (d, 2H), 2.22 (s, 3H), 1.28 (s, 12H).

According to the analysis of related databases, 17100-58-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; SMITHKLINE BEECHAM CORPORATION; WO2009/71504; (2009); A1;,
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