Extracurricular laboratory: Synthetic route of 2-Methyladamantan-2-ol

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.

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.702-98-7, name is 2-Methyladamantan-2-ol, molecular formula is C11H18O, molecular weight is 166.26, as common compound, the synthetic route is as follows.Recommanded Product: 702-98-7

A reactor made of glass was charged with 160 g of n-undecane, 80 g of 2-methyladamantanol, 4.1 g of methacrylic acid and 0.92 g of p-toluenesulfonic monohydrate. The resulting mixture was maintained for 1 hour while distilling off water under atmospheric pressure. Water was removed further by reflux at 120 C. for 1 hour under reduced pressure at 150 mmHg, whereby 2-methyladamantane was prepared. It was cooled to 0 C. A methacrylate forming reaction was then carried out by adding 103.6 g of methacrylic acid and 13.7 g of boron trifluoride ethyl ether to it while stirring the resulting mixture for 2 hours. After the reaction mixture was washed with 1275.5 g of a 10% aqueous sodium carbonate solution, followed by washing three times with 160 g of deionized water. In such a manner, 260 g of a n-undecane solution of 2-methyladamantan-2-yl methacrylate was obtained. The resulting solution contained 29.6 wt. % of 2-methyladamantan-2-yl methacrylate and 5.2 wt. % of 2-methyleneadamantane. The present invention was described specifically by using specific modes. It is however apparent for those skilled in the art that the present invention can be changed or modified without departing from the gist and scope of the present invention.

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; Mitsubishi Chemical Corporation; US2008/51597; (2008); A1;,
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Some tips on 3-Amino-1,1,1-trifluoropropan-2-ol

Statistics shows that 431-38-9 is playing an increasingly important role. we look forward to future research findings about 3-Amino-1,1,1-trifluoropropan-2-ol.

Related Products of 431-38-9, 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.431-38-9, name is 3-Amino-1,1,1-trifluoropropan-2-ol, molecular formula is C3H6F3NO, molecular weight is 129.0811, as common compound, the synthetic route is as follows.

3-Oxo-2-(pyridin-3-yl)-6-[4-(trifluoromethyl)phenyl]-2 ,3-di hydropyridazi ne-4-carboxylic acid (100 mg, 0.277 mmcl) was dissolved in anhydrous DMF (2.1 mL). (2RS)-3-Amino-1,1,1- trifluoropropan-2-ol (71.5 mg, 0.55 mmol), N-ethyl-N-isopropylpropan-2-amine (314 pL, 1.80mmol), and propane phosphonic acid anhydride (T3P, 243 pL, 50% in DMF, 415 pmol) were successively added. It was stirred at rt overnight. The reaction mixture was diluted with dichloromethane and concentrated under vacuum. The residue was purified by RP-HPLC (column: X-Bridge 018 5pm lOOx3Omm, mobile phase: (water + 0.2 vol% aqueous ammonia (32%)) acetonitrile, gradient) yielding 57.3 mg (44%) of the title compound.1H-NMR (400MHz, DMSO-d6): 6 [ppm] = 3.49 (ddd, 1H), 3.76 (ddd, 1H), 4.18-4.29 (m, 1H),6.68 (br s, 1H), 7.65 (ddd, 1H), 7.89 (d, 2H), 8.18 (ddd, 1H), 8.22 (d, 2H), 8.71 (dd, 1H), 8.75(s, 1H), 8.93 (d, 1H), 9.59 (t, 1H).

Statistics shows that 431-38-9 is playing an increasingly important role. we look forward to future research findings about 3-Amino-1,1,1-trifluoropropan-2-ol.

Reference:
Patent; BAYER AKTIENGESELLSCHAFT; BAYER PHARMA AKTIENGESELLSCHAFT; DEUTSCHES KREBSFORSCHUNGSZENTRUM; GUTCHER, Ilona; ROeHN, Ulrike; SCHMEES, Norbert; ZORN, Ludwig; ROeSE, Lars; BADER, Benjamin; KOBER, Christina; CARRETERO, Rafael; STOeCKIGT, Detlef; IRLBACHER, Horst; PLATTEN, Michael; (397 pag.)WO2018/146010; (2018); A1;,
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Extended knowledge of 5-Chloropentan-1-ol

At the same time, in my other blogs, there are other synthetic methods of this type of compound,5259-98-3, 5-Chloropentan-1-ol, and friends who are interested can also refer to it.

Adding a certain compound to certain chemical reactions, such as: 5259-98-3, 5-Chloropentan-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, COA of Formula: C5H11ClO, blongs to alcohols-buliding-blocks compound. COA of Formula: C5H11ClO

Intermediate 1; 4-(5-Chloro-pentyloxy)-benzoic acid methyl ester; 4-Hydroxy-benzoic acid methyl ester (1.52 g, 10 mmol), 5-chloro-l-pentanol (1.22 g, 10 mmol) and triphenylphosphine (2.62 g, 10 mmol) are dissolved in dry THF (30 rnL) and cooled to 0 0C. Diethylazodicarboxylate (DEAD) (1.74 g, 10 mmol) is dropped into this mixture at 0 ¡ãC and stirred at room temperature for 3 days. The reaction mixture is washed with brine, dried over Na2SO4, filtered and evaporated. The crude product is purified using silica-gel column chromatography (CH2CI2 only to CH2Cl2:2 M NH3 in MeOH=20:l) to give the desired product (1.14 g, 45percent). NMR (CDCI3): delta 7.98 (d, 2H , J = 8.8 Hz), 6.89 (d, 2H, / = 8.8Hz), 4.02 (t, 2H, J = 6.5 Hz), 3.88 (s, 3H), 3.57 (t, 2H, / = 6.7 Hz), 1.85 (m, 4H), 1.64 (m, 2H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,5259-98-3, 5-Chloropentan-1-ol, and friends who are interested can also refer to it.

Reference:
Patent; ELI LILLY AND COMPANY; WO2006/101808; (2006); A1;,
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A new synthetic route of 6214-44-4

The synthetic route of 6214-44-4 has been constantly updated, and we look forward to future research findings.

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. 6214-44-4, name is (4-Ethoxyphenyl)methanol, the common compound, a new synthetic route is introduced below. Computed Properties of C9H12O2

To a solution of (4-ethoxyphenyl)methanol (300 mg, 1.971 mmol, commercial source: Apollo SCI) and triethylamine (328 muIota_, 2.365 mmol) in Dichloromethane (15 mL) at 0C, methanesulfonyl chloride (168 muIota_, 2.168 mmol) was added dropwise. The mixture was stirred at 0 C for 3 h. Upon completion, the reaction mixture was diluted with water and DCM and extracted with DCM (2x20ml). The combined organic layers were dried over anh. MgS04 and filtered. The filtrate was concentrated under reduced pressure to obtain 4-ethoxybenzyl methanesulfonate (454 mg, 100%) This product was used without any purification in the next reaction.

The synthetic route of 6214-44-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GLAXOSMITHKLINE INTELLECTUAL PROPERTY DEVELOPMENT LIMITED; ALEMPARTE-GALLARDO, Carlos; ENCINAS, Lourdes; ESQUIVIAS PROVENCIO, Jorge; (206 pag.)WO2019/34729; (2019); A1;,
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Introduction of a new synthetic route about [1,1′-Biphenyl]-3-ylmethanol

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,69605-90-9, its application will become more common.

Reference of 69605-90-9, 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. 69605-90-9, name is [1,1′-Biphenyl]-3-ylmethanol. A new synthetic method of this compound is introduced below.

General procedure: Oxidation of alcohols was typically carried out as follows: a suspension with 5 mg of the synthesized catalyst in acetonitrile (2 mL) was magnetically stirred, and the substrate namely alcohols (0.1 mmol) and PhIO (2.5 equiv.) was then added. The resulting mixture was kept at 60 C with magnetical stirring for a set time. The selectivity and conversion were determined by GC analysis.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,69605-90-9, its application will become more common.

Reference:
Article; Yang, Zhi-Wang; Zhao, Xia; Li, Tian-Jing; Chen, Wen-Long; Kang, Qiao-Xiang; Xu, Xue-Qing; Liang, Xi-Xi; Feng, Ying; Duan, Huan-Huan; Lei, Zi-Qiang; Catalysis Communications; vol. 65; (2015); p. 34 – 40;,
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Analyzing the synthesis route of 4464-18-0

According to the analysis of related databases, 4464-18-0, the application of this compound in the production field has become more and more popular.

Synthetic Route of 4464-18-0, 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 4464-18-0, name is Benzene-1,3,5-triyltrimethanol. This compound has unique chemical properties. The synthetic route is as follows.

As asolution A, 16.8 g (0.1 mol) of 1,3,5-tris (hydroxymethyl) benzene and 0.32 g (0.5 mmol) of dibutyltin EGI-1 (2-methacryloyloxyethyloxy) ethyl isocyanate was changed to a solution in which dilaurate was dissolved and the addition amount of 2- (2-methacryloyloxyethyloxy) ethyl isocyanate was changed to 61.8 g (0.31 mol) EGI-6 (76.2 g, yield 99%) was obtained by synthesizing in the same manner as in the synthesis procedure of EGI-6.The dataof1H NMR spectrum ofthe obtained EGI-6were as follows.

According to the analysis of related databases, 4464-18-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; TOKUYAMA DENTAL CORPORATION; SUZUKI, TAKESHI; SAKATA, EIBU; YAMAGAWA, JUN-ICHIRO; (25 pag.)JP6225054; (2017); B2;,
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The important role of 4541-14-4

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, 4541-14-4, 4-(Benzyloxy)butan-1-ol.

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. 4541-14-4, name is 4-(Benzyloxy)butan-1-ol. A new synthetic method of this compound is introduced below., HPLC of Formula: C11H16O2

To stirred solution of alcohol 21 (10 g, 55.5 mmol) in dichloromethane (150 mL) at 0 C were added pyridinium chlorochromate (17.96 g, 83.33 mmol) and Celite (17.96 g) and stirred at room temperature for 5 h. Diethyl ether (100 mL) was added and the reaction mixture was filtered through a small pad of Celite and silica gel. The filtered cake was washed thoroughly with ether (2 ¡Á 150 mL) and the filtrate was concentrated under reduced pressure. After flash column chromatography on silica gel (100-200 mesh, eluent: 8% EtOAc in hexane) aldehyde 22 (9.09 g, 92%) was obtained as a colorless liquid. 1H NMR (400 MHz, CDCl3): delta 9.76 (t, J = 1.5 Hz, 1H), 7.36-7.17 (m, 5H), 4.46 (s, 2H), 3.47 (q, J = 5.1 Hz, 2H), 2.53 (td, J = 7.0, 1.5 Hz, 2H), 1.92 (ddd, J = 13.0, 7.0, 6.0 Hz, 2H); 13C NMR (75 MHz, CDCl3): delta 201.3, 138.2, 128.4, 127.6, 73.0, 69.0, 41.0, 22.6; MASS (EIMS): m/z 178 (M)+.

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, 4541-14-4, 4-(Benzyloxy)butan-1-ol.

Reference:
Article; Venkatesham, Akkaladevi; Nagaiah, Kommu; Tetrahedron Asymmetry; vol. 23; 15-16; (2012); p. 1186 – 1197,12;,
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Share a compound : N-(2-Hydroxyethyl)ethylenediamine

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,111-41-1, its application will become more common.

Adding a certain compound to certain chemical reactions, such as: 111-41-1, N-(2-Hydroxyethyl)ethylenediamine, 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, 111-41-1, blongs to alcohols-buliding-blocks compound. Recommanded Product: N-(2-Hydroxyethyl)ethylenediamine

1), synthesis:To a 500 ml three-necked flask was added 104 g of hydroxyethyl ethylenediamine (1.0 mol), 94.7 g of paraformaldehyde (3 mol, 95%), stirred for 30 minutes, and at room temperature of 80-90 C 156.8 g of formic acid (3 mol, ), About 1 hour dropping end, continue to control the temperature of 80-90 C for 1 hour. 70g (vacuum-0.094MPa, kettle temperature: 80C) was distilled off under reduced pressure. The product was analyzed by gas chromatography at a concentration of 91.8% and 8% of the impurity S-2 (i.e., by-product N, N, N’-trimethyl-N’-ethylidene-ethylenediamine).2), transesterification:100 g of n-butanol was added to the three-necked flask of step 1) and the temperature was raised to 120 C for 4 hours to effect the reaction of the by-product N, N, N’-trimethyl-N’-ethylidene- Ammonia transesterification reaction to produce TMAEEA, by gas chromatography analysis, impurity S-2 content of 0.05%, after cooling back.3), distillation purification:The liquid of step 2) was transferred to a 500 ml rectification flask under reduced pressure at a vacuum of -0.094 MPa, a component at 62 C was n-butanol and a transesterified n-butanolate, 118 C component Ie product TMAEEA. A mixture of 139 g at 118 C was collected, the yield was 95.2% and the content was 99.9%.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,111-41-1, its application will become more common.

Reference:
Patent; Sichuan Zhijiang High-tech Materials Co., Ltd.; Zhang Qi; Zhang Chao; Zhang Hua; Ye Xiaoming; Chen Xinzhi; (7 pag.)CN106748826; (2017); A;,
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New learning discoveries about 3,4-Dichlorobenzyl alcohol

With the rapid development of chemical substances, we look forward to future research findings about 1805-32-9.

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 1805-32-9, name is 3,4-Dichlorobenzyl alcohol. This compound has unique chemical properties. The synthetic route is as follows. Formula: C7H6Cl2O

General procedure: The solution of the crude 6D’ and Ph3PHBr (2.16 g, 6.3mmol) in CH3CN was refluxed overnight. Evaporation ofthe reaction mixture yielded 2.25 g of crude compound 7D’ as a white solid in 76% yield (2 steps) and used for the next reaction without further purification

With the rapid development of chemical substances, we look forward to future research findings about 1805-32-9.

Reference:
Article; Kim, Sung-Soo; Fang, Yuanying; Park, Haeil; Bulletin of the Korean Chemical Society; vol. 36; 6; (2015); p. 1676 – 1680;,
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Extended knowledge of 4728-12-5

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,4728-12-5, its application will become more common.

Synthetic Route of 4728-12-5, In the chemical reaction process,reaction time,type of solvent,can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product.An updated downstream synthesis route of 4728-12-5 as follows.

To a suspension of sodium hydride (0.41 g, 10.26 mmol, 60percent in mineral oil) in tetrahydrofuran (15 mL), (2,2-dimethyl-1,3-dioxan-5-yl)methanol (1 , 1 g, 6.84 mmol) was added and the reaction mixture was stirred at room temperature for 10 min. Then methyl iodide (1 .27 mL, 20.52 mmol) was added drop wise at room temperature and the reaction mixture was stirred at room temperature for 6 h. The reaction mixture was quenched with ice water (15 mL) and extracted with ethyl acetate (2 x 30 mL). The combined organic layer was dried over anhydrous sodium sulphate, filtered and concentrated. The crude was purified by silica gel column chromatography using 60percent ethyl acetate in hexane to afford the title compound 5-(methoxymethyl)-2,2-dimethyl-1,3-dioxane (2, 0.65 g, 60percent yield) as a colorless oil. _ NMR (400 MHz, CDCI3) _ (ppm): 3.97-3.93 (m, 2H), 3.76-3.72 (m, 2H), 3.42 (d, J = 6.8 Hz, 2H), 3.34 (s, 3H), 2.00-1 .94 (m, 1H), 1 .42 (s, 3H), 1 .40 (s, 3H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,4728-12-5, its application will become more common.

Reference:
Patent; CADENT THERAPEUTICS; ANDERSON, David, R.; VOLKMANN, Robert, A.; MENNITI, Frank; FANGER, Christopher; XU, Yuelian; (252 pag.)WO2018/119374; (2018); A1;,
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