Category: alcohols-buliding-blocks

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. 6161-87-1, name is 2-(2,4,6-Trichlorophenoxy)ethanol. A new synthetic method of this compound is introduced below., Quality Control of 2-(2,4,6-Trichlorophenoxy)ethanol

EXAMPLE 3 Preparation of 2-(2,4,6-trichlorophenoxy)-ethyl chloride Into a three-necked, round-bottom flask fitted with a stirrer, thermometer, reflux condenser and dropping funnel was added 250 g of 96% 2-(2,4,6-trichlorophenoxy) ethanol, 250 ml carbon tetrachloride and 4 g of benzyl-trimethyl-ammonium chloride. The mixture was heated to 55 C. and 146 g thionyl chloride was added dropwise over 1.5 hours. After the addition of the thionyl chloride the temperature of the reaction was slowly raised to 80 C. for a total reaction tme of 2.5 to 3 hours. The end of the reaction was determined by GLC. The mixture was cooled to 60 C. and water slowly added to decompose the excess thionyl chloride. The phases were separated and the organic phase was washed with a 10% sodium hydroxide solution until it reached a pH of 7. After an additional separation of the phases the organic phase was washed again with water. After a further separation of phases, the carbon tetrachloride was distilled off to yield an oil which slowly crystallized to form 257 g of 2-(2,4,6-trichlorophenoxy)-ethyl chloride in a purity of 96%-98% and yield of 98%.

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, 6161-87-1, 2-(2,4,6-Trichlorophenoxy)ethanol.

Reference:
Patent; Makhteshim Chemical Works Ltd.; US5091578; (1992); A;,
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Adding a certain compound to certain chemical reactions, such as: 100058-61-5, 3-(Benzyloxy)cyclobutanol, 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, Product Details of 100058-61-5, blongs to alcohols-buliding-blocks compound. Product Details of 100058-61-5

Preparation of 3-(benzyloxy)cyclobutyl sulfochloridate (CC): A solution of compound BB (1.7 g, 9.53 mmol) in DCM (100 ml) was treated with triethylamine (3.34 ml, 23.84 mmol) followed by MeSO2Cl (MsCl) (1.47 ml, 19.07 mmol) and stirred at 25 C. for 30 minutes. The reaction mixture was poured into water and extracted with DCM. The organic layer was dried over Na2SO4, filtered, and concentrated to provide crude CC. Yield: 3.5 g. 1H NMR (400 MHz, CDCl3): 7.36-7.27 (m, 5H), 4.67-4.60 (m, 1H), 4.42 (s, 2H), 3.76-3.69 (m, 1H), 2.97 (s, 3H), 2.85-2.78 (m, 2H), 2.35-2.28 (m, 2H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,100058-61-5, 3-(Benzyloxy)cyclobutanol, and friends who are interested can also refer to it.

Reference:
Patent; Pfizer Inc; US2008/280879; (2008); A1;,
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Related Products of 20605-01-0 ,Some common heterocyclic compound, 20605-01-0, molecular formula is C9H16O6, 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.

General procedure: A solution of diethyl 2,2-bis(hydroxymethyl) malonate(12 mmol), 1 (10 mmol) and sulfonated carbon(1.0 g) were heated to reflux in a mixture of N,N-dimethylformamide(10 mL) and cyclohexane (6 mL)under stirring for 3 h. After cooling to room temperature,the solution was filtered and the solvent was removed in vacuo, the residue was dissolved in EtOAc (15 mL),washed with saturated brine (10 mL × 2) and water(10 mL×2), dried over anhydrous Na2SO4. The solventwas filtered and concentrated to give 2a-2d as colorless oil.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,20605-01-0, its application will become more common.

Reference:
Article; Yuan, Lin; Li, Zhong Yan; Zhang, Min; Yuan, Xian You; Zhu, Xiao Qing; Journal of Nanoscience and Nanotechnology; vol. 17; 3; (2017); p. 2201 – 2205;,
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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. 647-42-7, name is 3,3,4,4,5,5,6,6,7,7,8,8,8-Tridecafluorooctan-1-ol. A new synthetic method of this compound is introduced below., category: alcohols-buliding-blocks

To a mixture, kept under stirring, of C6F13CH2CH2OH(252 g, 0.692 moles), tetrahydrofurane (350 ml) and cyclohexane (300 ml) at 250C, an aqueous solution ofNaOH (400 ml, 50%) was added drop-wise. After stirring for 2 hours, benzyltriethyl ammonium chloride (25 g, 0.11 moles) as phase transfer catalyst, and then 1- bromopentane (209 g, 1.38 moles) were added. The reaction mixture was kept under stirring at 400C for 40 hours, then at 700C for 8 hours. The resulting mixture was poured into water and the organic phase thus ob- tained was washed two times with water. After removing the fraction having a low boiling point, the raw product was subjected to distillation at reduced pressure, thus obtaining 215 g of C6F13CH2CH2O (CH2) 4CH3 (yield 72%, boiling point 110C/6 mbar, n 1.3385) . Spectrographic data confirm the obtained structure: GC/MS m/z at 435 (M+H)+, 377 (M-CH2CH2CH2CH3) +, 71 (- CH2CH2CH2CH2CH3) + ; for NMR data see Tables 1-2.

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, 647-42-7, 3,3,4,4,5,5,6,6,7,7,8,8,8-Tridecafluorooctan-1-ol.

Reference:
Patent; ALChiMI.A. S.r.l.; WO2009/133575; (2009); A1;,
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Adding a certain compound to certain chemical reactions, such as: 34626-51-2, 5-Bromopentan-1-ol, 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: 5-Bromopentan-1-ol, blongs to alcohols-buliding-blocks compound. Recommanded Product: 5-Bromopentan-1-ol

To a solution of 5-bromopentan-1-ol (0.43 mL, 3.00 mmol) in tetrahydrofuran (15 mL) at 0 C under an atmosphere of nitrogen was added imidazole (210 mg, 3.00 mmol) and t-butylchlorodiphenylsilane (0.78 mL, 3.00 mmol) at 0 C. After 5 h at room temperature, the reaction mixture was quenched by addition of water (5 mL) and the mixture was extracted with diethyl ether. The organic layer was washed with brine, dried over magnesium sulfate, filtered and evaporated in vacuo. The resulting crude residue was purified on a Biotage purification apparatus (silica gel, 0-10% ethyl acetate in hexanes gradient) to yield the title compound (17, 980 mg, 2.42 mmol, 81%) as a colorless oil. 1H NMR (400 MHz, CDCl3) delta 7.72-7.69 (m, 4H), 7.48-7.39 (m, 6H), 3.70 (t, J = 6.4 Hz, 1H), 3.42 (t, J = 6.8 Hz, 1H), 1.91-1.84 (m, 2H), 1.62-1.58 (m, 2H), 1.47-1.42 (m, 4H), 1.09 (s, 9H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,34626-51-2, 5-Bromopentan-1-ol, and friends who are interested can also refer to it.

Reference:
Article; Kim, Min Ju; Lee, Suk Ho; Park, So Ok; Kang, Hyunku; Lee, Jun Sung; Lee, Ki Nam; Jung, Myung Eun; Kim, Jeongmin; Lee, Jinhwa; Bioorganic and Medicinal Chemistry; vol. 19; 18; (2011); p. 5468 – 5479;,
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Adding a certain compound to certain chemical reactions, such as: 2568-33-4, 3-Methylbutane-1,3-diol, 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 3-Methylbutane-1,3-diol, blongs to alcohols-buliding-blocks compound. Safety of 3-Methylbutane-1,3-diol

To a solution of ethyl (2E) -3- (2-{ [3-chloro-5- (trifluoromethyl)pyridin-2-yl]oxy}-4-hydroxyphenyl) acrylate (10.0 g) in tetrahydrofuran (300 ml) were added tributylphosphine (10.5 ml), 3-methylbutane-l, 3-diol (4.0 ml) and 1, 1′ – (azodicarbonyl) dipiperidine (9.7,6 g) , and the mixture was stirred overnight at 500C. Then, tributylphosphine (10.5 ml), 3-methylbutane-l, 3-diol (4.0 ml) and 1,1′- (azodicarbonyl) dipiperidine (9.76 g) were added, and the mixture was stirred at 500C for 1 hr. The reaction mixture was concentrated, the obtained solid was washed with diisopropyl ether, and the filtrate was concentrated. The obtained residue was subjected to basic silica gel column chromatography, and eluted with ethyl acetate-hexane (hexane alone to 45:55, v/v). The obtained residue was subjected to silica gel column chromatography, and eluted with ethyl acetate-hexane (hexane alone to 3:7, v/v) to give ethyl (2E) -3- [2-{ [3-chloro-5- (trifluoromethyl)pyridin-2-yl]oxy}-4- (3-hydroxy-3- methylbutoxy) phenyl] acrylate (Reference Example 264) (1.46. g, yield: 12-%) ,as a pale-yellow solid. Recrystallization from ethyl acetate-hexane gave white crystals as 0.5 hydrate, melting point 63.5-66.00C.Then, ethyl (2E) -3- [2-{ [3-chloro-5-(trifluoromethyl) pyridin-2-yl] oxy}-4- (3-hydroxy-l, 1- dimethylpropoxy) phenyl] acrylate (Reference Example 265) (0.71 g, yield: 6%) was obtained as an orange oil.1H-NMR (300 MHz, DMSO-ds)delta: 1.20 (3 H, t, J = 7,2 Hz), 1.32 (6 H, s), 1.87 (2 H, t, J = 7.5 Hz), 3.55 – 3.62 (2 H, m) , 4.12 (2 H, q, J = 7.2 Hz), 4.40 (1 H, t, J = 5.4 Hz), 6.57 (1 H, d, J = 16.2 Hz), 6.96 (1 H, s) , 6.94 – 6.99 (1 H, m) , 7.55 (1 H, d, J = 16.2 Hz), 8.50 – 8.50 (1 H, m) , 8.63 (1 H, d, J = 2.0 EPO Hz ) .

At the same time, in my other blogs, there are other synthetic methods of this type of compound,2568-33-4, 3-Methylbutane-1,3-diol, and friends who are interested can also refer to it.

Reference:
Patent; TAKEDA PHARMACEUTICAL COMPANY LIMITED; WO2007/18314; (2007); A2;,
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Electric Literature of 1074-61-9 , The common heterocyclic compound, 1074-61-9, name is (4-Vinylphenyl)methanol, molecular formula is C9H10O, 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.

Step A 1-Bromomethyl-4-vinyl-benzene. Bromine (16.4 g, 103 mmol) was slowly added to a solution of triphenylphosphine (28.87 g, 110.1 mmol) in CH2Cl2 (260 mL) at 0 C. After 10 minutes, 4-vinylbenzyl alcohol (12.5 g, 93.3 mmol) was added and the reaction mixture was stirred at 0 C. for 2 h. The reaction mixture was washed with water (1*) followed by brine (1*). The organic solution was dried over MgSO4, filtered, and concentrated in vacuo. The product was triturated with petroleum ether (3*), and the ethereal solution was concentrated in vacuo. The residue was purified by flash chromatography (hexanes) to afford 4-vinyl-benzyl bromide (6.23 g). 1H NMR (400 MHz, CDCl3) delta 7.32-7.45 (m, 4H), 6.72 (dd, 1H), 5.77 (d, 1H), 5.28 (d, 1H), 4.50 (s, 2H).

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

Reference:
Patent; Pfizer Inc.; US6288120; (2001); B1;,
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Reference of 46190-45-8, 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. 46190-45-8, name is Methyl 4-(2-hydroxyethyl)benzoate. A new synthetic method of this compound is introduced below.

Step 3 4-(2-Phenoxy-ethyl)-benzoic Acid Methyl Ester 72 4-(2-Hydroxyethyl)benzoic acid methyl ester 71 (1.622 g, 9.00 mmol), triphenyl phosphine (3.541 g, 13.50 mmol), and diethyl azodicarboxylate (2.13 ml, 13.50 mmol) were dissolved in 50 ml of tetrahydrofuran at room temperature and allowed to stir for 30 minutes. Phenol (0.847 g, 9.00 mmol) was added and the mixture was allowed to stir overnight. The mixture was diluted with water and extracted with diethyl ether. The extracts were dried over anhydrous sodium sulfate and concentrated en vacuo. The residue was purified by flash chromatography on silica eluted with 99:1 hexane/acetone to give 387 mg (16.8%) of 4-(2-phenoxy-ethyl)-benzoic acid methyl ester 72 as a clear oil.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,46190-45-8, Methyl 4-(2-hydroxyethyl)benzoate, and friends who are interested can also refer to it.

Reference:
Patent; Cournoyer, Richard Leo; Keitz, Paul Francis; Lowrie Jr., Lee Edwin; Muehldorf, Alexander Victor; O’Yang, Counde; Yasuda, Dennis Mitsugu; US2001/56100; (2001); A1;,
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Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 24131-31-5, name is (3,5-Bis(benzyloxy)phenyl)methanol. This compound has unique chemical properties. The synthetic route is as follows. category: alcohols-buliding-blocks

Phosphorus tribromide was added to the CH2Cl2 solution (10 mL) of [3,5-bis(benzyloxy)phenyl]methanol (11, 0.008 mol) at 0 C for 2 h. Ice water was added to reaction solution, and extracted with diethyl ether. The crude product was evaporated and purified by silica-gel chromatography using petroleum/ethyl acetate 15:1 as an eluent to give bromide 12 (0.0028 mol, 35%). 1H-NMR (DMSO-d6, 300 MHz) delta: 7.11-7.43 (10H), 6.65 (2H, d, J = 2.1 Hz), 6.55 (1H, s), 5.03 (4H, br s), 4.35 (2H, s). HPLC analysis 96.9% (MeOH: H2O = 85: 15 (V/V), tR = 8.67 min).

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, 24131-31-5, (3,5-Bis(benzyloxy)phenyl)methanol.

Reference:
Article; Wan, Xiang; Wang, Xiao-Bing; Yang, Ming-Hua; Wang, Jun-Song; Kong, Ling-Yi; Bioorganic and Medicinal Chemistry; vol. 19; 17; (2011); p. 5085 – 5092;,
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Related Products of 575-03-1, 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 575-03-1, name is 7-Hydroxy-4-(trifluoromethyl)coumarin. This compound has unique chemical properties. The synthetic route is as follows.

General procedure: The appropriate bromoketone (6a-o) (1.7 mmol) and triethylamine (1.6 mmol) were added to as olution of either7-hydroxy-4-methyl-2H-chromen-2-one 4 (1.4 mmol)or 7-hydroxy-4-(trifluoromethyl)-2H-chromen-2-one 5 (1.4 mmol) in THF (20 mL). The mixture was stirred at room temperature for 24h, filtered and the solvent was evaporated under reduced pressure.The solid residue was purified by column chromatography eluting with DCM/MeOH 9:1 to afford (7a-n) and (8a-o).

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 575-03-1, 7-Hydroxy-4-(trifluoromethyl)coumarin.

Reference:
Article; Kandil, Sahar; Westwell, Andrew D.; Mcguigan, Christopher; Bioorganic and Medicinal Chemistry Letters; vol. 26; 8; (2016); p. 2000 – 2004;,
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