Tag: M.W=100-200

Related Products of 100058-61-5, 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. 100058-61-5, name is 3-(Benzyloxy)cyclobutanol. A new synthetic method of this compound is introduced below.

To a solution of anti-3-(benzyloxy)cyclobutan-1-ol (3.65 mmol, 650 mg) in dry DMF (8 mL) was added 60% sodium hydride(5.47 mmol, 1.5 equiv.) portion wise at 0 C. After the mixture was stirred at 0 C for 15 min, iodomethane (7.29 mmol, 454 muL) was added dropwise at 0 C. The reaction mixture was stirred at room temperature (~ 25 C) for 1-2 h. The mixture was quenched with saturated aqueous of NH4Cl (10 mL), diluted with water (20 mL), extracted with ethyl acetate (20 mL × 2), washed with brine (20 mL), the organic layer was concentrated under reduced pressure, and the crude product was purified by column chromatography on silica gel (petroleum ether/ethyl acetate = 60:1 as eluent) to give ((anti-3-methoxycyclobutoxy) methyl) benzene (513 mg, 73 % yield) as colorless oil.

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:
Article; Sheng, Ren; Yang, Liu; Zhang, Yanchun; Xing, Enming; Shi, Rui; Wen, Xiaoan; Wang, Heyao; Sun, Hongbin; Bioorganic and Medicinal Chemistry Letters; vol. 28; 15; (2018); p. 2599 – 2604;,
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Related Products of 3562-73-0, 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. 3562-73-0, name is 1-(4-Biphenylyl)ethanol, molecular formula is C14H14O, 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.

General procedure: In a typical reaction, alcohol (0.4 mmol) was mixed with AlCl3 (0.02 mmol, 5 mol%) and triphenylphosphine (PPh3, 0.02 mmol, 5 mol%) in nitromethane (1.0 mL). Thereafter the mixture was stirred at 80 C for 2 h. After the reaction, the mixture was cooled to room temperature, and the product was isolated using preparative thin layer chromatography (TLC, eluting solution: petroleum ether/ethyl acetate, 5/1 (v/v)). Tests for substrate scope were all performed with an analogous procedure.

According to the analysis of related databases, 3562-73-0, the application of this compound in the production field has become more and more popular.

Reference:
Article; Liu, Changhui; Pan, Bin; Gu, Yanlong; Cuihua Xuebao/Chinese Journal of Catalysis; vol. 37; 6; (2016); p. 979 – 986;,
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Adding a certain compound to certain chemical reactions, such as: 702-98-7, 2-Methyladamantan-2-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, HPLC of Formula: C11H18O, blongs to alcohols-buliding-blocks compound. HPLC of Formula: C11H18O

COMPARATIVE EXAMPLE 1 Synthesis of 2-methyl-2-adamantyl alpha-trifluoromethylacrylate [MAFAC] from 2-methyl-2-adamantanol and alpha-trifluoromethylacryloyl Chloride A 500 ml flask was flushed with nitrogen to displace the air with nitrogen, and was charged with 83.1 g (0.50 mol) of 2-methyl-2-adamantanol, 101.2 g (1.0 mol) of triethylamine and 200 g of tetrahydrofuran. Then 118.9 g (0.75 mol) of alpha-trifluoromethylacryloyl chloride was dropwise added to the content in the flask over a period of about 1 hour, while the content was maintained at a reaction temperature of about 0 C. Then the content was stirred for 10 hours at room temperature. After completion of the reaction, the reaction mixture was washed with water and then with an aqueous saturated sodium chloride solution. The thus-obtained organic phase was subjected to column chromatography, and further, analyzed by NMR and mass spectrometry. Thus, 101.2 g (yield: 70.3%) of the object 2-methyl-2-adamantyl alpha-trifluoromethylacrylate was obtained.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,702-98-7, 2-Methyladamantan-2-ol, and friends who are interested can also refer to it.

Reference:
Patent; TOSOH CORPORATION; US2003/139613; (2003); A1;,
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Application of 1205037-95-1, 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 1205037-95-1, name is trans-3-Aminocyclobutanol hydrochloride. This compound has unique chemical properties. The synthetic route is as follows.

In an ice bath, 25.4 mg (0.635 mmol) sodium hydride (60% dispersion in mineral oil) were dispensed in 2 mL of anhydrous THF. 52.9 mg (0.43 mmol) trans-3- aminocyclobutanol hydrochloride in 2 mL of a 1 : 1 mixture of anhydrous DMF and anhydrous THF were slowly added. After complete addition, stirring at 0C was continued for 15 min. 100 mg (0.287 mmol) of 6-chloro-3-(5-methoxy-1 -benzofuran- 2-yl)imidazo[1 ,2-b]pyridazine were added, the ice bath was removed and the resulting mixture was stirred for 72 h at 40 C. The reaction mixture was cooled to rt and a freshly prepared mixture of 9 mg (0.225 mmol) sodium hydride (60% dispersion in mineral oil) and 18 mg (0.146 mmol) trans-3-aminocyclobutanol hydrochloride in 1 mL of a 1 : 1 mixture of anhydrous DMF and anhydrous THF were added to the reaction mixture. Stirring at 40 C was continued for 18 h. The reaction mixture was carefully poured into water. The aqueous layer was extracted with ethyl acetate. The combined organic layers were dried over magnesium sulfate, and concentrated. The crude product was purified by HPLC to give 54 mg of the title compound as a solid material. 1H-NMR (300 MHz, DMSO-d6), delta [ppm] = 2.53 (4H), 3.68-3.77 (1 H), 3.79 (3H), 5.47- 5.58 (1 H), 6.90 (1 H), 7.00 (1 H), 7.26 (1 H), 7.48-7.57 (2H), 8.09-8.17 (2H). LC-MS (Method 3): Rt = 0.76 min; MS (ESIpos) m/z = 351 [M+H]+.

According to the analysis of related databases, 1205037-95-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Bayer Intellectual Property GmbH; EIS, Knut; PUeHLER, Florian; ZORN, Ludwig; SCHOLZ, Arne; LIENAU, Philip; GNOTH, Mark, Jean; BOeMER, Ulf; GUeNTHER, Judith; HITCHCOCK, Marion; WO2013/34570; (2013); A1;,
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Related Products of 7287-81-2, 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. 7287-81-2, name is 1-(m-Tolyl)ethanol, molecular formula is C9H12O, 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.

To 1 mL of a 0 C. 0.3M solution of the corresponding aryl fluoride in tetrahydrofuran ?THF? (0.3 mmol) was added 0.6 mL of a 1 M solution of potassium t-butoxide in THF (0.6 mmol) and 0.3 mL of a 1 M solution of the corresponding alcohol (0.3 mmol) in THF. The resultant mixtures were shaken and allowed to warm to room temperature over approximately 72 hours. The solvent was removed in vacuo using a Genevac HT-12 to obtain a sample that was then purified by reverse phase HPLC.

According to the analysis of related databases, 7287-81-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Pfizer Inc; US2009/170886; (2009); A1;,
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Related Products of 440-60-8, 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. 440-60-8, name is (Perfluorophenyl)methanol, molecular formula is C7H3F5O, 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.

At 100mL2.95g (25mmol) of 2,3,4,5,6-pentafluorobenzyl alcohol was added to the three-necked flask.Triethylamine 2.5g,Toluene 40mL,Slow dropCis-2,2-dimethyl-3-(E/Z-2-chloropropenyl)cyclopropanecarboxylic acid chloride 6g (29mmol),The reaction was carried out at room temperature for 4 hours.The organic phase is sequentially 20mL5% sodium hydroxide solution,Wash with 5% hydrochloric acid solution and saturated sodium chloride solution, dry,After desolvation, a pale yellow viscous liquid is obtained.After column chromatography (petroleum ether / ethyl acetate = 20/1), 9.0 g of pale yellow liquid was obtained.The yield was 96%.

According to the analysis of related databases, 440-60-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Mt. Huang College; Han Bingbing; Zheng Zubiao; (15 pag.)CN109776327; (2019); A;,
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Related Products of 111-45-5, 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.111-45-5, name is 2-(Allyloxy)ethanol, molecular formula is C5H10O2, molecular weight is 102.13, as common compound, the synthetic route is as follows.

Sodium hydroxide (2.56 g, 63.99 mmol) was completely dissolved in distilled water and a solution of THF and Allyloxy ethanol (5.83 ml, 54.55 mmol) was added at 0 C. After stirring for 30 minutes, a solution of 4-Toluenesulfonyl chloride (10 g, 52.45 mmol) in THF at 0 C was slowly added. After that, the temperature was raised to room temperature and then stirred for 1 hour. The reaction was terminated by adding cold distilled water and extracted with hexane. The extracted organic layer was washed with water and aqueous NaCl solution, and dried over MgSO4. The reaction product (1EO-OTs) was dried in a vacuum oven (Yield = 33%).

Statistics shows that 111-45-5 is playing an increasingly important role. we look forward to future research findings about 2-(Allyloxy)ethanol.

Reference:
Patent; Korea Research Institute of Chemical Technology; Han Mi-jeong; Kang Yeong-gu; Seok Jeong-don; Kwak Hyeon-ju; (29 pag.)KR101826496; (2018); B1;,
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Electric Literature of 52273-77-5, 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.52273-77-5, name is 2-(3-Aminophenyl)ethanol, molecular formula is C8H11NO, molecular weight is 137.179, as common compound, the synthetic route is as follows.

In a glass reaction flask are combined 73 grams of sublimed quinizarin (available from Aceto Corp., Lake Success, N.Y.), 49 grams of leucoquinizarin (available from Aceto Corp.), 66 grams of 3-aminobenzene ethanol (available from Frinton Labs, Vineland, N.J.), 31 grams of boric acid (available from Aldrich Chemical Co., Milwaukee, Wis.), and 780 grams of methanol (available from J T Baker, Phillipsburg, N.J.). The materials are mixed and heated until the solvent refluxes at about 66 C. After about 16 hours of reflux, it is believed that the reaction will be complete, having generated an alcohol-substituted colorant of the formula [CHEMMOL-00109] [0194] The reaction mixture is cooled and filtered. The product filter cake is dried in air at ambient temperature. The spectral strength of the alcohol-substituted colorant is determined using a spectrophotographic procedure based on the measurement of the colorant in solution by dissolving the colorant in toluene and measuring the absorbance using a Perkin Elmer Lambda 2S UV/VIS spectrophotometer. The spectral strength of the alcohol-substituted colorant is believed to be measured as about 21,000 mL Absorbance Units per gram at absorption lambdamax.

Statistics shows that 52273-77-5 is playing an increasingly important role. we look forward to future research findings about 2-(3-Aminophenyl)ethanol.

Reference:
Patent; Xerox Corporation.; US2004/82801; (2004); A1;,
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Reference of 29683-23-6 , The common heterocyclic compound, 29683-23-6, name is Tetrahydro-2H-thiopyran-4-ol, molecular formula is C5H10OS, 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.

The compound obtained in (80 mg, 0.28 mmol), tetrahydro-2H-thiopyran-4-ol (33.1 mg, 0.28 mmol) and triphenylphosphine (110.2 mg, 0.42 mmol) were dissolved in THF (2.5 mL), which was then slowly added with diethyl azodicarboxylate (DEAD, 191 muL, 0.42 mmol) and stirred at room temperature for 19 hours. The resulting mixture was concentrated and purified by silica gel chromatography to obtain the title compound (white solid, 33.7 mg, 31% yield). 1H NMR (300 MHz, CDCl3) delta 8.02 (d, 1H), 7.97 (dd, 1H), 7.18 (d, 1H), 6.79 (d, 1H), 6.67 (d, 1H), 4.50 – 4.38 (m, 3H), 3.91 (s, 3H), 3.00 – 2.92 (m, 2H), 2.87 – 2.76 (m, 1H), 2.63 – 2.47 (m, 3H), 2.36 (s, 3H), 2.27 – 2.17 (m, 2H), 2.12 – 2.01 (m, 2H)

The synthetic route of 29683-23-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SK Chemicals Co., Ltd.; LEE, Ju Young; LEE, Jeong A; AHN, Jaeseung; RYU, Je Ho; HAN, Min-Young; YOO, Taekyung; SA, Joon Ho; KIM, Jae-Sun; (297 pag.)EP2963027; (2016); A1;,
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Synthetic Route of 675580-49-1, 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. 675580-49-1, name is (6-Chloroimidazo[1,2-b]pyridazin-3-yl)methanol. A new synthetic method of this compound is introduced below.

To a solution of (6-chloro-imidazo[1 ,2-b]pyridazin-3-yl)-methanol (1.3 g, 7.1 mmol) in DCM (50 ml_) was added active MnO2 (3 g, 34.5 mmol). The mixture was stirred at rt overnight and filtered. The filtrate was concentrated under vacuum and the residue was washed with EtOAc to affrode 6-chloro-imidazo[1 ,2-b]pyridazine-3-carbaldehyde (0.7 g) in 54% yield. 1H- NMR (400MHz, CDCI3) delta ppm 10.36 (s, 1 H), 8.42 (s, 1 H), 8.08 (d, 1 H), 7.38 (d, 1 H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,675580-49-1, (6-Chloroimidazo[1,2-b]pyridazin-3-yl)methanol, and friends who are interested can also refer to it.

Reference:
Patent; NOVARTIS AG; DAI, Miao; FU, Xingnian; HE, Feng; JIANG, Lei; LI, Yue; LIANG, Fang; LIU, Lei; MI, Yuan; XU, Yao-chang; XUN, Guoliang; YAN, Xiaoxia; YU, Zhengtian; ZHANG, Ji, Yue; WO2011/20861; (2011); A1;,
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