Author: tianli

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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Electric Literature of 149104-89-2, 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.149104-89-2, name is (4-Bromo-3-methylphenyl)methanol, molecular formula is C8H9BrO, molecular weight is 201.06, as common compound, the synthetic route is as follows.

To a solution of (4-bromo-3-methyl-phenyl)methanol (45.0 g, 224 mmol) in dichloromethane (500 mL) were sequentially added imidazole (38.1 g, 559 mmol) and tert-butyldimethylsilyl chloride (40.5 g, 269 mmol) and the reaction mixture was stirred at ambient temperature for 15 hours. The mixture was washed with water (2*500 mL), saturated NaCl (500 mL) and dried over anhydrous sodium sulfate. The dried solution was filtered and concentrated to give (4-bromo-3-methyl-phenyl)methoxy-tert-butyl-dimethyl-silane (68.0 g, 96.4% yield) as a brown oil. 1H NMR (CDCl3, 400 MHz) delta 7.48 (d, J=8.2 Hz, 1H), 7.19 (d, J=1.1 Hz, 1H), 7.02 (dd, J=1.6, 8.1 Hz, 1H), 4.67 (s, 2H), 2.40 (s, 3H), 0.95 (s, 9H), 0.11 (s, 6H).

The chemical industry reduces the impact on the environment during synthesis 149104-89-2, I believe this compound will play a more active role in future production and life.

Reference:
Patent; Celgene Corporation; Alexander, Matthew D.; Carrancio, Soraya; Correa, Matthew D.; Grant, Virginia Heather Sharron; Hansen, Joshua; Harris, Roy L.; Huang, Dehua; Kercher, Timothy S.; Lopez-Girona, Antonia; Nagy, Mark A.; Plantevin-Krenitsky, Veronique; (115 pag.)US2019/322647; (2019); A1;,
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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 624-95-3, name is 3,3-Dimethylbutan-1-ol. This compound has unique chemical properties. The synthetic route is as follows. Computed Properties of C6H14O

[00056] Example I represent a reference oxidation reaction under the conditions analogous to the one (reported in J.Organic Chemistry, 1987, 52, 2559 and J. Organic Chemistry, 1989, 54, 2970), also known as Anelli protocol. [00057] 820 mg of 3,3-Dimethyl-1-butanol (8 mmol) and 14.9 mg MeO-TEMPO (0.08 mmol) are dissolved in toluene (20 cc) in a jacketed glass reaction flask, equipped with a thermocouple, an addition port, a Teflon coated magnetic stir bar and a pH probe. Potassium bromide (45.25 mg, 0.4 mmol) and 1310 mg of NaHCO3 are dissolved in water (21.6 cc) and the aqueous phase is added to the stirred organic fraction at 1000 RPM in the reaction flask. The stirred suspension is cooled to 0 C. and 5.4 g of 12.3% aqueous NaOCl (8.92 mmol) are added via a gas-tight syringe over 5 minutes. The reaction mixture is aged for an additional 30 min and the organic layer sampled for GC assay. The yield of 3,3-dimethylbutyraldehyde is 77% at 30 min and 91% at 60 min reaction time

With the rapid development of chemical substances, we look forward to future research findings about 624-95-3.

Reference:
Patent; The NutraSweet Company; US6825384; (2004); B1;,
Alcohol – Wikipedia,
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Application of 597-31-9, 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. 597-31-9, name is 3-Hydroxy-2,2-dimethylpropanal, molecular formula is C5H10O2, 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 a solution of N-(2-(difluoromethoxy)-6-methylpyridin-3-yl)-3-(2-isopropylphenyl)azetidine-3-carbox-amide Ex 3 (68 mg, 0.18 mmol) and 3-hydroxy-2,2-dimethyl-propanal (25 mg, 0.245 mmol) in MeOH (2 mL) under inert atmosphere is added sodium cyanoborohydride (18 mg, 0.29 mmol). The reaction mixture is stirred at 50C for 2 h (reaction monitored by LCMS) and is then quenched with water (2 mL). The mixture is diluted with MeCN (2 mL) and is then purified by prep. HPLC (Prep-HPLC-3 conditions) to give the title compound Ex 11-17 (46 mg, 55% yield) as a colorless glass. LCMS-1 : tR = 0.79 min, [M+1]+ 462.41; 1H NMR (500 MHz, CDC )<5: 8.61 (d, J = 8.1 Hz, 1 H), 8.07 (s, 1 H), 7.42-7.35 (m, 3 H), 7.33-7.29 (m, 1 H), 7.19 (d, J = 7.7 Hz, 1 H), 6.92 (d, J = 8.1 Hz, 1 H), 4.25 (s br, 2 H), 3.70 (s br, 2 H), 3.50 (s, 2 H), 2.60 (s, 2 H), 2.53-2.45 (m, 1 H), 2.39 (s, 3 H), 1.14 (d, J = 6.7 Hz, 6 H), 0.94 (s, 6 H). According to the analysis of related databases, 597-31-9, the application of this compound in the production field has become more and more popular. Reference:
Patent; IDORSIA PHARMACEUTICALS LTD; BOLLI, Martin; BROTSCHI, Christine; LESCOP, Cyrille; WILLIAMS, Jodi T.; (0 pag.)WO2019/234115; (2019); A1;,
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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 111-46-6, name is 2,2′-Oxybis(ethan-1-ol). This compound has unique chemical properties. The synthetic route is as follows. Application In Synthesis of 2,2′-Oxybis(ethan-1-ol)

In steel esterification reactor with the volume of 15 1 equipped with a heating element and a stirring device, 3550 g of benzoic acid, 1500 g of diethylene glycol are charged, 13 g of titanium (IV) isopropoxide are added. Before the heating treatment, xylene in the amount of 2500 g is added to separator. The reaction is conducted at the constant feed of xylene into the reaction mass by the circulating pump from the separator with the rate of 3 1/hour. The reaction mass is heated to the temperature 200C, in an hour after the beginning of the heating the temperature is raised to 220C, in two hours after the beginning of the heating the temperature is raised to 240C. In 3 hours after the beginning of the heating the pressure in. reactor is reduced to 15 kPa, in 30 min more the pressure in reactor is reduced to 5 kPa. In 4 hours after the beginning of the heating the reaction mass is cooled. From the esterification reactor 4400 g of reaction mass comprising 0.5% by weight of benzoic acid, 0.3 % by weight of diethylene glycol benzoate and 99.0% by weight of diethylene glycol dibenzoate are discharged. From the separator an aqueous phase comprising 785 g of water, 8 g of benzoic acid, as well as organic phase comprising 1720 g of xylene, 365 g of benzoic acid, is discharged.

With the rapid development of chemical substances, we look forward to future research findings about 111-46-6.

Reference:
Patent; PUBLIC JOINT STOCK COMPANY “SIBUR HOLDING”; NOSIKOV, Aleksei Aleksandrovich; BABIN, Ivan Anatolievich; POPOVTSEV, Egor Evgenievich; IGASHEVA, Varvara Petrovna; (28 pag.)WO2019/59801; (2019); A1;,
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