Author: tianli

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.35373-63-8, name is 2-Amino-3-(4-chlorophenyl)propan-1-ol, molecular formula is C9H12ClNO, molecular weight is 185.6507, as common compound, the synthetic route is as follows.Quality Control of 2-Amino-3-(4-chlorophenyl)propan-1-ol

In addition to the foregoing, numerous other chromatographic separations using a column bonded with a CSP including a derivatized cyclofructan residue were carried out. Tables 5-9 list some additional examples of chromatographic separations using a column bonded with a CSP of the present invention. AU examples of chromatographic separations using columns bonded with CSPs of the present invention were carried out using the following experimental conditions and procedures.|0132| The high performance liquid chromatography (HPLC) column packing system was composed of an air driven fluid pump (HASKEL, DSTV- 122), an air compressor, a pressure regulator, a low pressure gauge, two high-pressure gauges (10,000 and 6,000 psi), a slurry chamber, check valves, and tubings. The CSPs were slurry packed into a 25 cm x 0.46 cm (inner diameter, I. D.) stainless steel column.|0133| The HPLC system was an Agilent 1 100 system (Agilent Technologies, Palo Alto,CA), which consisted of a diode array detector, an autosampler, a binary pump, a temperature- controlled column chamber, and Chemstation software. All chiral analytes were dissolved in ethanol, methanol, or other appropriate mobile phases, as indicated. For the LC analysis, the injection volume and flow rate were 5 muL and 1 mL/min, respectively. Separations were carried out at room temperature (~20 0C) if not specified otherwise. The wavelengths of UV detection were 195, 200, 210, and 254 nm. The mobile phase was degassed by ultrasonication under vacuum for 5 min. Each sample was analyzed in duplicate. Three operation modes (the normal phase mode, polar organic mode, and reversed phase mode) were tested, unless indicated otherwise. In the normal phase mode, heptane with ethanol or isopropanol was used as the mobile phase. In some cases, trifluoroacetic acid (TFA) was used as an additive, as indicated. The mobile phase of the polar organic mode was composed of acetonitrile/methanol and small amounts of acetic acid and triethylamine. Water/acetonitrile or acetonitrile/acetate buffer (20 mM, pH = 4.1 ) was used as the mobile phase in the reversed-phase mode.|0134| Two different supercritical fluid chromatographic instruments were used. One was a Berger SFC unit with an FCM 1200 flow control module, a TCM 2100 thermal column module, a dual pump control module, and a column selection valve. The flow rate was 4 mL/min. The cosolvent was composed of methanol/ethanol/isopropanol = 1 : 1 : 1 and 0.2% diethylamine (DEA). The gradient mobile phase composition was 5% cosolvent hold during 0- 0.6 min, 5-60% during 0.6-4.3 min, 60% hold during 4.3-6.3 min, 60%-5% during 6.3-6.9 min, and 5% hold during 6.9-8.0 min. The other SFC system was a Jasco (MD, USA) system comprised of an autosampler unit (AS-2059-SF Plus), a dual pump module (PU-2086 Plus), a column thermostat module (CO-2060 Plus), a UV/Vis detector (UV-2075 Plus), and a back pressure regulator module (SCH-Vch-BP). Unless otherwise specified, the mobile phase was composed of CCVmethanol (0.1 % TFA or 0.1% diethylamine). The flow rate was 3 mL/min.|0135| For the calculations of chromatographic data, the “dead time” to was determined by the peak of the refractive index change due to the sample solvent or determined by injecting l ,3,5-tri-/e/-/-butylbenzene in the normal phase mode.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,35373-63-8, 2-Amino-3-(4-chlorophenyl)propan-1-ol, and friends who are interested can also refer to it.

Reference:
Patent; BOARD OF REGENTS, THE UNIVERSITY OF TEXAS SYSTEM; ARMSTRONG, Daniel, W.; PING, Sun; BREITBACH, Zachary, S.; WANG, Chunlei; WO2010/148191; (2010); A2;,
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Adding a certain compound to certain chemical reactions, such as: 4442-79-9, 2-Cyclohexylethanol, 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, 4442-79-9, blongs to alcohols-buliding-blocks compound. HPLC of Formula: C8H16O

General procedure: The alcohol (1.0 eq) was added to a suspension of Dess-Martin periodinane (1.2 eq) in CH2Cl2(100 mM) under an argon atmosphere at room temperature. The mixture was allowed to stir for0.5 – 20 hours, while consumption of starting material was monitored by TLC. After the reactionwas complete, 1M Na2S2O3 (equal volume to CH2Cl2) was added. After stirring for 15 minutes,the phases were separated and the aqueous phase was extracted with CH2Cl2 twice. Thecombined organic layers were washed with 5% NaHCO3 and brine, and dried over Na2SO4. Thesolvent was evaporated under reduced pressure and the residue was purified by columnchromatography to afford analytically pure aldehydes.b) alcohol precursors for aldehydes 13, 14, 20 (solid alcohols)The alcohol (1.0 eq) was dissolved in CH2Cl2 (200 mM) and the solution was added to asuspension of Dess-Martin periodinane (1.2 eq) in CH2Cl2 (200 mM) under an argon atmosphereat room temperature. The mixture was allowed to stir for 0.5 – 20 hours (TLC monitoring). Then,Et2O (equal volume to CH2Cl2), 1M Na2S2O3 and saturated NaHCO3 (both equal volume toCH2Cl2) were added. After stirring for 15 minutes, the phases were separated and the aqueousphase was extracted with Et2O twice. The combined organic layers were washed with sat.NaHCO3 and brine, and dried over Na2SO4. The solvent was evaporated under reduced pressureand the residue was purified by column chromatography to afford analytically pure aldehydes.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,4442-79-9, its application will become more common.

Reference:
Article; Ruff, Bettina M.; Braese; O’Connor, Sarah E.; Tetrahedron Letters; vol. 53; 9; (2012); p. 1071 – 1074;,
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Application of 19064-18-7 ,Some common heterocyclic compound, 19064-18-7, molecular formula is C7H6F2O, 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.

15.5 ml (15.5 mmol) of a 1M solution of potassium tert-butoxide in tetrahydrofuran at 0 C was added to a solution of 1.72 ml (15.5 mmol) (2,6-difluorophenyl) methanol and 1.6 ml (15.5 mmol) 4-bromo-2-fluoropyridine in 50 ml of anhydrous tetrahydrofuran.The reaction mixture was stirred at room temperature for 18 h.It was partitioned between ethyl acetate and water.The organic phase was separated and washed with water and saturated aqueous sodium chloride solution, dried, filtered and concentrated over sodium sulfate.The residue was purified by chromatography on silica gel (40 g silica gel cartridge, mobile phase: cyclohexane / ethyl acetate, gradient 0% to 100%) purified.This gave 4.12 g of the target compound (88% d. Th.).

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. 19064-18-7, (2,6-Difluorophenyl)methanol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BAYER PHARMA AKTIENGESELLSCHAF; VAKALOPOULOS, Alexandros; FOLLMANN, Markus; BUCHGRABER, Philipp; HARTUNG, Ingo; LINDNER, Niels; WUNDER, Frank; STASCH, Johannes-Peter; MARQUARDT, TOBIAS; REDLICH, Gorden; DIETZ, Lisa; LI, Volkhart Min-Jian; (391 pag.)TW2016/5850; (2016); A;,
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Adding a certain compound to certain chemical reactions, such as: 10488-69-4, Ethyl 4-chloro-3-hydroxybutanoate, 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: 10488-69-4, blongs to alcohols-buliding-blocks compound. Recommanded Product: 10488-69-4

In a three-necked flask, 200 mL of tetrahydrofuran and 19 g of diisopropylamine were added and cooled to -10 ° C. 134 mL of n-butyllithium was added slowly while keeping the temperature, and the mixture was stirred for 30 minutes. The internal temperature of the reactor was maintained at -40 to -30 , 36 mL of tert-butyl acetate was slowly added dropwise, and the mixture was stirred for 1 hour while maintaining the temperature of the reaction solution. (S) -ethyl 4-chloro-3-hydroxybutanoate was added dropwise at -40 to -30 ° C for 30 minutes and stirred for 30 minutes. The inner temperature of the reaction solution was raised naturally to -20 to -10 ° C The reaction was then completed by further stirring for 2 hours. When the reaction is complete, waterAnd the reaction was quenched. To the reaction solution was added 300 mL of ethyl acetate. The reaction mixture was stirred for 30 minutes to extract the product. The organic layer was extracted and separated. The organic layer was treated with anhydrous magnesium sulfate, filtered and concentrated under reduced pressure The obtained oily product (12.3 gr) was obtained.

The synthetic route of 10488-69-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Nebula Pharma PVT. LTD; Jang, Myung Sik; Jang, Rae Kyu; Mo, Gil Wung; Jung, In Hwa; Lee, In Kyu; Han, Ka Ram; (25 pag.)KR101528359; (2015); B1;,
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Reference of 6240-11-5, 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. 6240-11-5, name is 1-Adamantaneethanol. A new synthetic method of this compound is introduced below.

EXAMPLE 19 1-Adamantaneethanol (10 g, 0.05 mol), 4-hydroxyphenylacetic acid (8.43 g, 0.05 mol) and p-toluenesulfonic acid (1 g, 0.006 mol) were refluxed in benzene (100 mL) with continuous water separation for 8 hours, then allowed to stir overnight. The residue was washed, first with 5% aqueous sodium bicarbonate solution (50 mL) and then twice with water (50 mL), then was dried over anhydrous MgSO4 and filtered. The filtrate was concentrated in vacuo. The product, (adamant-1-yl)ethyl 4-hydroxyphenylacetate, was taken up in epichlorohydrin (50 mL) and refluxed for 2 hours in the presence of DBU (1 mL, 0.007 mol).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,6240-11-5, 1-Adamantaneethanol, and friends who are interested can also refer to it.

Reference:
Patent; Bodor; Nicholas S.; US4829086; (1989); A;,
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Electric Literature of 932-01-4, 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 932-01-4, name is 4,4-Dimethylcyclohexanol. This compound has unique chemical properties. The synthetic route is as follows.

Method A: To a solution of 4,4-dimethylcyclohexanol (100 mg, 0.78 mmol) and Et3N (201 mg, 1.56 mmol) in CH2C12 (2 mL) was added methanesulfonyl chloride (178 mg, 1.56 mmol) at 0C and the reaction mixture was stirred at rt for 2 h before it was quenched with water and was extracted with CH2C12. The organic layer was washed with brine, separated, dried, filtered and concentrated to afford 4,4-dimethylcyclohexyl methanesulfonate which was used without further purification. To a solution of 7-nitrophthalazin-l(2H)-one (Intermediate- 10, step-1 , 100 mg, 0.52 mmol) in THF (2 mL) was added NaH (41 mg, 1.02 mmol, 60% in mineral oil) at 0C and stirred for 15 minutes. Then a solution of 4,4-dimethylcyclohexyl methanesulfonate in THF (1 mL) was slowly added to the reaction mixture at 0C. Then the reaction mixture was heated at 80C for 6 h before it was quenched with water and was extracted with EtOAc. The organic layer was washed with brine, separated, dried, filtered and concentrated. The residue was purified by column chromatography to afford 180 mg of the title product/H NMR (300 MHz, DMSO d6): delta 9.27 (s, 1H), 8.59-8.56 (d, / = 8.7 Hz, 1H), 8.30 (s, 1H), 7.88-7.85 (d, / = 8.7 Hz, 1H), 4.97-4.93 (m, 1H), 2.08-1.99 (m, 2H), 1.72-1.67 (m, 2H), 1.57-1.43 (m, 4H), 1.04 (s, 3H), 0.99 (s, 3H).

According to the analysis of related databases, 932-01-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; GLENMARK PHARMACEUTICALS S.A.; GHARAT, Laxmikant Atmaram; BANERJEE, Abhisek; KHAIRATKAR-JOSHI, Neelima; KATTIGE, Vidya Ganapati; WO2013/72825; (2013); A1;,
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Related Products of 702-82-9, Adding some certain compound to certain chemical reactions, such as: 702-82-9, name is 3-Aminoadamantan-1-ol,molecular formula is C10H17NO, 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 702-82-9.

27.6 g (0.30 mol, 1.5 eq) of glyoxylic acid monohydrate,3-amino-1-adamantanol 33.5 g (0.20 mol, 1.0 eq),38.8 g (0.30 mol, 1.5 eq) of diisopropylethylamine and 250 g of tetrahydrofuran were placed in the reaction flask.51.1 g (0.50 mol, 2.5 eq) of acetic anhydride was added dropwise.Heat and reflux for 2 hours.The remaining amount of controlled raw materials in HPLC is less than 1%.Add 50g of water and stir for 30 minutes.Layered,The aqueous layer was extracted once with 50 g of dichloromethane.The organic layer was concentrated under reduced pressure to give a white solid.Compound II 42.8g,The yield is 96.1%.Purity 96.6%

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. 702-82-9, 3-Aminoadamantan-1-ol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Dalian Zhengbang Information Advisory Co., Ltd.; Gao Feng; Xie Nan; (7 pag.)CN108503571; (2018); A;,
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Adding a certain compound to certain chemical reactions, such as: 2425-41-4, (2-Phenyl-1,3-dioxane-5,5-diyl)dimethanol, 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, name: (2-Phenyl-1,3-dioxane-5,5-diyl)dimethanol, blongs to alcohols-buliding-blocks compound. name: (2-Phenyl-1,3-dioxane-5,5-diyl)dimethanol

The monobenzalpentaerythritol (5.00 g, 22.3 mmol), (3.5) 12G1-C02H (4b) (24.07 g, 49.05 mmol), and DPTS (5.90 g, 22.3 mmol) were dissolved in anhydrous CH2C12 (120 mL). DCC (1 1.96 g, 57.97 mmol) dissolved in anhydrous CH2C12 (20 mL) was added and the reaction was stirred for 12 h. at room temperature under nitrogen atmosphere. After the reaction was complete, the mixture was diluted, filtered, and rinsed with Et20. The solvent was removed and the crude product was purified by column chromatography (Si02, 5% Et20:hexane) and followed by precipitation in MeOH to give a white solid as a product: 25.29 g (97%). XH NMR (500 MHz, CDC13) delta 7.55 – 7.46 (m, 2H, PhH-3, 5), 7.41 – 7.34 (m, 3Eta, PhH-2, 4, 6), 7.12 (d, J= 2.3 Hz, 2H, ArH-2, 6), 7.1 1 (d, J= 2.2 Hz, 2H, ArH-2′, 6′), 6.64 (t, J= 2.2 Hz, 1H, ArH-4), 6.62 (t, J= 2.2 Hz, 1H, ArH-4′), 5.52 (s, 1Eta, CH-acetal), 4.82 (s, 2Eta, ArC02CH2), 4.33 (d, J= 11.8 Hz, 2H, 20CHaHb-ring), 4.26 (s, 2H, ArC02CH2), 4.03 (d, J= 11.8 Hz, 2H, 20CHaHb-ring), 3.98 – 3.90 (m, 8Eta, 4ArOCH2), 1.81 – 1.73 (m, 8Eta, 4ArOCH2CH2), 1.48 – 1.40 (m, 8Eta, 4ArOCH2CH2CH2), 1.26 (m, 64Eta, 4(CH2)8CH3), 0.88 (t, J= 6.9 Hz, 12H, 4CH3). 13C NMR (126 MHz, CDC13) delta 166.3 (C=0), 166.2 (C=0′), 160.4 (ArC-3, 5), 160.3 (ArC-3 ‘, 5’), 137.8 (PhC-1), 131.7 (PhC-3, 5), 131.2 (PhC-4), 129.4 (PhC-2, 6), 128.5 (ArC-1), 126.3 (ArC-1 ‘), 107.89 (ArC-2, 6), 107.85 (ArC-2′, 6′), 106.81 (ArC-4), 106.5 (ArC- 4′), 102.4 (CH-acetal), 69.9 (OC-ring), 68.52 (ArOCH2), 68.49 (ArOCH2′), 64.2 (ArC02CH2), 63.5 (ArC02CH2’), 38.0 (C(CH20)4), 32.1 (CH2CH2CH3), 29.82, 29.79, 29.76, 29.73, 29.6, 29.5, 29.3, 26.2 (ArOCH2CH2CH2), 22.8 (CH2CH3), 14.3 (CH3). The spectroscopic data of 16b are in agreement with those previously reported.

The synthetic route of 2425-41-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; PERCEC, Virgil; WO2014/190024; (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.4719-04-4, name is 2,2′,2”-(1,3,5-Triazinane-1,3,5-triyl)triethanol, molecular formula is C9H21N3O3, molecular weight is 219.2813, as common compound, the synthetic route is as follows.Computed Properties of C9H21N3O3

To 50.0 g(0.228 mol) of hexahydrotriazine (I) was added undervigorous agitation at 0C 16.14 g (0.114 mol) of P2O5until a homogeneous mass was formed. The resultingmixture was heated to 80C for 1 h. A 66.0-g (96%) portionof a light yellow viscous fl uid was obtained. Found,%: C 36.18, H 7.38, N 14.21. C9H22N3O6. Calculated,%: C 36.12, H 7.41, N 14.04, , 10.35.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,4719-04-4, 2,2′,2”-(1,3,5-Triazinane-1,3,5-triyl)triethanol, and friends who are interested can also refer to it.

Reference:
Article; Ishmiyarov; Rakhimova; Latypova; Abdullin; Voloshin; Dokichev; Russian Journal of Applied Chemistry; vol. 88; 7; (2015); p. 1174 – 1177; Zh. Prikl. Khim. (S.-Peterburg, Russ. Fed.); vol. 88; 7; (2015); p. 1083 – 1086,4;,
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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. 17100-58-2, name is (4-Bromo-2-methylphenyl)methanol. A new synthetic method of this compound is introduced below., Recommanded Product: 17100-58-2

[0653j To a solution of (4-bromo-2-methylphenyl)methanol (1.3 g, 6.7 mmol) in CH2C12 (50 mL) was added PBr3 (0.95 mL, 10 mmol) at 0 C. The mixture was stirred at rt for 1 h, quenched with ice-water (50 mL) and the pH value was adjusted to 7.0 with 50% aqueous NaOH solution. The mixture was extracted with EtOAc (100 mL x 2) and the combined organic layers were washed with water (50 mL), dried (Na2SO4) and concentrated in vacuo to give 4-bromo-1- (bromomethyl)-2-methylbenzene (1.56 g, yield: 89%) as a white solid which was used in next step without further purification.

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, 17100-58-2, (4-Bromo-2-methylphenyl)methanol.

Reference:
Patent; BIOGEN IDEC MA INC.; SUNESIS PHARMACEUTICALS, INC.; HOPKINS, Brian, T.; MA, Bin; CHAN, Timothy, Raymond; SUN, Lihong; ZHANG, Lei; KUMARAVEL, Gnanasambandam; LYSSIKATOS, Joseph, P.; KOCH, Kevin; MIAO, Hua; WO2015/89337; (2015); A1;,
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