Month: May 2021

Application of 116-02-9 ,Some common heterocyclic compound, 116-02-9, molecular formula is C9H18O, 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.

1, equipped with a stirrer, condensate return pipe, thermometer, N.2The four-necked flask was purged with nitrogen and the addition of acrylic acid and 3,3,5-trimethylcyclohexanol, the molar ratio of acrylic acid to 3,3,5-trimethylcyclohexanol was 1: 1.2, , Stirring speed of 300 r / min, heating up; 2, continue to heat up to 118 , stable condensate reflux, adding catalyst, incubation reaction 4h; and then remove the condenser, install the water separator, at 125 reaction 3h, stop And then distilled at a temperature of 80 C and a pressure of -0.099 MPa to obtain a pale yellow transparent product with an acrylic acid conversion of 94.6% and a yield of 85.14%.The catalyst is p-toluenesulfonic acid in an amount of 1.0% by weight based on the total weight of the total reactants.

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. 116-02-9, 3,3,5-Trimethylcyclohexanol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; SOUTH CHINA UNIVERSITY OF TECHNOLOGY; PAN, CHAOQUN; ZHANG, JIN; KANG, YINGZI; (6 pag.)CN104151159; (2016); B;,
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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. 756520-66-8, name is 1-(2,6-Dichloro-3-fluorophenyl)ethanol, the common compound, a new synthetic route is introduced below. name: 1-(2,6-Dichloro-3-fluorophenyl)ethanol

Dissolve triphenylphosphine (17.50g, 66.73mmol) in THF,Argon protection, injection under ice bathDEAD (10.57mL, 66.73mmol),Add 1-(2,6-dichloro-3-fluorophenyl)ethanol (9.30g, 44.49mmol)And m-bromophenol (5.19mL, 48.94mmol) in THF,Move to room temperature and react overnight. TLC monitors the reaction is complete,The solvent was distilled off under reduced pressure,Separation and purification by silica gel column chromatography (petroleum ether / dichloromethane =200: 1, v / v) to obtain a transparent oil (8.51g, yield 52.84%).

The synthetic route of 756520-66-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Chinese Academy Of Sciences Shanghai Pharmaceutical Institute; Chinese Academy Of Sciences Shanghai Life Sciences Institute; Liu Hong; Yang Chenghua; Li Chunpo; Sun Chenxia; Liang Xuewu; Gao Yang; Shi Yuqiang; Zhao Sen; Jiang Hualiang; Chen Kaixian; (34 pag.)CN110950807; (2020); A;,
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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. 162744-59-4, name is (4-Bromo-2,6-difluorophenyl)methanol, the common compound, a new synthetic route is introduced below. Recommanded Product: (4-Bromo-2,6-difluorophenyl)methanol

Example 2 1: 4~((7~ (4-chloro-3-metho. xyphenvl)-l-(4-fl orophenvl)~4,5,6, 7~tetrahvdro~ IH-benzofd, Yitnldazo Patent; JANSSEN PHARMACEUTICA NV; ZHANG, Xuqing; WALL, Mark; SUI, Zhihua; WO2015/160772; (2015); A1;,
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Synthetic Route of 1462-03-9, 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. 1462-03-9, name is 1-Methylcyclopentanol. A new synthetic method of this compound is introduced below.

E11-1 : Potassium cyanide (1. 43 g, 22.0 mmol) was added to a stirred solution of METHYLCYCLOPENTANOL (2.00 g, 20.0 MMOL) in glacial acetic acid (1.00 mL) resulting in a thick slurry. To this was added, dropwise, sulfuric acid (3 mL, caution: exothermic) at a rate at which the temperature was maintained at ca. 30-35C. Additional acetic acid (1 mL) was added to facilitate stirring of the thick paste. The mixture was then heated to 55-60C for 30 min followed by stirring at ambient temperature for 16 h. Ice cold water (35 mL) was then added, the mixture extracted with ethyl ether (2x 40 mL) and the combined organic phases washed with 5% NAHCO3 (5x 30 mL), dried over MGS04 and the solvent evaporated to yield a pale brown oil (1.16 g). The pH of the combined aqueous washings was then raised to pH 11 by the addition of solid K2CO3 AND the resulting solids filtered and washed with ethyl ether (3x 40 mL). The filtrate was extracted with ethyl ether (2x 40 mL), the combined extracts dried over MgS04 and the solvent evaporated to yield additional product (0.355 g) which was combined with the above obtained oil (1.52 g, 60 %).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,1462-03-9, its application will become more common.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; BOEHRINGER INGELHEIM PHARMA GMBH & CO KG; WO2004/103996; (2004); A1;,
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Adding a certain compound to certain chemical reactions, such as: 6850-39-1, 3-Aminocyclohexanol, 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: 6850-39-1, blongs to alcohols-buliding-blocks compound. Recommanded Product: 6850-39-1

To a stirred solution of 3-aminocyclohexanol (40.0 g, 0.348 mol) in DCM (350 ml) were added imidazole (71.0 g, 1.042 mol) and TBDMS-C1 (78.0 g, 0.520 mol) at 0 C. The mixture was allowed to stir at RT for 24 h. The reaction was quenched by H20, extracted with DCM, washed with brine solution, dried, filtered and concentrated to give title compound. Yield 78.1 g (crude); [M+H]+ = 230.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,6850-39-1, 3-Aminocyclohexanol, and friends who are interested can also refer to it.

Reference:
Patent; ORION CORPORATION; WOHLFAHRT, Gerd; RUMMAKKO, Petteri; KARJALAINEN, Arja; PASSINIEMI, Mikko; PIETIKAeINEN, Pekka; HAIKARAINEN, Anssi; VAeISAeNEN, Emilia; TIAINEN, Eija; WO2014/202827; (2014); A1;,
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Application of 454-91-1, 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 454-91-1, name is 1-[3-(Trifluoromethyl)phenyl]ethanol. This compound has unique chemical properties. The synthetic route is as follows.

Example 3-1 Synthesis of O-{1-(3-trifluoromethylphenyl)ethyl}-acetohydroxamate A 20 mg portion of DMF was added to 5 ml of toluene solution containing 3 g (15.8 mmol) of 1-(3-trifluoromethylphenyl)ethylalcohol. Then, 2.25 g (18.9 mmol) of thionyl chloride was added under ice-cooling. After 2 hours of stirring at 10C or less, this was concentrated under a reduced pressure on a water bath at temperature of 50 to 60C. After cooling to room temperature, 8 ml of DMF, 3.3 g (23.9 mmol) of anhydrous potassium carbonate and 2.15 g (20.5 mmol) of acetohydroxamic acid were added, and the mixture was stirred for 6 hours while heating at 120 to 130C. After cooling, ethyl acetate was added to the reaction mixture, and the mixture was washed with water and saturated brine in that order and then dried over anhydrous sodium sulfate. This was concentrated under a reduced pressure, and the resulting residue was purified by a silica gel column chromatography (n-Hex:AcOEt = 1:1 ? 1:2) to give 2.32 g of the title compound (yield = 59.5%). Melting point; 75.3 – 76.5C 1H-NMR delta (CDCl3); 1.57 (3H, d), 1.8 – 2.2 (3H, br), 4.8 – 5.15 (1H, br), 7.45 – 7.55 (4H, m), 7.8 – 8.0 (1H, br)

According to the analysis of related databases, 454-91-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; MITSUBISHI CHEMICAL CORPORATION; EP949243; (1999); A1;,
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Adding a certain compound to certain chemical reactions, such as: 27129-87-9, (3,5-Dimethylphenyl)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, Computed Properties of C9H12O, blongs to alcohols-buliding-blocks compound. Computed Properties of C9H12O

Example 174 Synthesis of methyl 3-[4-(3,5-dimethylphenylmethyloxy)-3-(1H-indol-5-yl)-phenyl]Propionate (Compound No. 174) (Preparation Method 5, Step e-2) A solution of Intermediate 55 (80 mg) and TMAD (69 mg, TCI) in anhydrous THF (1.5 ml) was added with 3,5-dimethylbenzyl alcohol (59 mul, Ald), added dropwise with nBu3P (110 mul, KANTO) under ice cooling, gradually warmed to room temperature and stirred for 13 hours.The reaction mixture was filtered, and the solvent of the filtrate was evaporated under reduced pressure.The residue was purified by column chromatography (Quad, hexane:ethyl acetate=7:1) to obtain the title compound (Compound No. 174, 123 mg).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,27129-87-9, (3,5-Dimethylphenyl)methanol, and friends who are interested can also refer to it.

Reference:
Patent; Shoda, Motoshi; Kuriyama, Hiroshi; US2004/44258; (2004); A1;,
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Related Products of 5299-60-5, 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. 5299-60-5, name is Ethyl 6-hydroxyhexanoate, molecular formula is C8H16O3, 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: To a solution of donor (1 mmol) in dry CH2Cl2 (5-10 ml) was added under argon ethyl 6-hydroxy-hexanoate (1.5 mmol) and 4 A molecular sieves (mass = donor + acceptor weight) then the mixture was stirred for 15 min. N-Iodosuccinimide (3 mmol) and trifluoromethanesulfonic acid (0.3 mmol) were successively added and after stirring 30 min at room temperature, the mixture was diluted with CH2Cl2, filtered on a celite pad and washed with satd aq NaHCO3 and satd aq Na2S2O3. The aqueous layer was extracted with CH2Cl2 then the combined organic layers were dried (MgSO4), filtered and concentrated. The residue was purified by flash chromatography.

According to the analysis of related databases, 5299-60-5, the application of this compound in the production field has become more and more popular.

Reference:
Article; Despras, Guillaume; Robert, Raymond; Sendid, Boualem; MacHez, Emeline; Poulain, Daniel; Mallet, Jean-Maurice; Bioorganic and Medicinal Chemistry; vol. 20; 5; (2012); p. 1817 – 1831;,
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Application of 647-42-7, 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. 647-42-7, name is 3,3,4,4,5,5,6,6,7,7,8,8,8-Tridecafluorooctan-1-ol, molecular formula is C8H5F13O, 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.

A succinic anhydride (9.7 g, 49 mmol), tetrahydrofuran (10 ml), and triethylamine (0.2 mL) were added to 2-(perfluorohexyl)ethanol (33.3 g, 46 mmol). A reaction was allowed for 60 min at an increased temperature of 100C while stirring the mixture. Water (100 mL) was added after cooling the mixture to 30C, and the precipitated crystals formed upon further cooling to 15C were filtered off to obtain carboxylic acid (5a; 39.7 g, 94%).

According to the analysis of related databases, 647-42-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; FUJIFILM Corporation; MIZUMURA Masatoshi; KATOH Shunya; UEMURA Minoru; ISHIWATAYasuhiro; YOSHIKAWA Masaru; MATSUYAMA Hiroshi; EP2738155; (2014); A1;,
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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.60666-70-8, name is (2-Bromo-5-chlorophenyl)methanol, molecular formula is C7H6BrClO, molecular weight is 221.48, as common compound, the synthetic route is as follows.Recommanded Product: 60666-70-8

Synthesis of l-bromo-4-chloro-2-(methoxymethyl)benzene 6c [00180] To a solution of (2-bromo-5-chloro-phenyl)methanol (3.16 g, 14.25 mmol) in THF (50 mL) at room temperature was added sodium hydride (684 mg, 17.10 mmol). The mixture was stirred for 30 min and then iodomethane (3.04 g, 1.33 mL, 21.38 mmol) was added and the reaction stirred overnight. The mixture was diluted with saturated aqueous ammonium chloride and EtOAc and the organic washed with water, then brine, and dried ( a2S04) and concentrated to afford the title compound 6c as an oil (3.36 g, quant). XH NMR (500 MHz, CDC13) delta 7.40 – 7.48 (2H, m), 7.1 1 – 7.14 (1H, m), 4.47 (2H, s), 3.48 (3H, s).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,60666-70-8, (2-Bromo-5-chlorophenyl)methanol, and friends who are interested can also refer to it.

Reference:
Patent; VERTEX PHARMACEUTICALS INCORPORATED; BOYALL, Dean; DAVIS, Christopher; DODD, James; EVERITT, Simon; MILLER, Andrew; WEBER, Peter; WESTCOTT, James; YOUNG, Stephen; WO2014/81689; (2014); A1;,
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