Month: May 2021

Reference of 17087-50-2, 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 17087-50-2 as follows.

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.

According to the analysis of related databases, 17087-50-2, the application of this compound in the production field has become more and more popular.

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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Synthetic Route of 887267-47-2, 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. 887267-47-2, name is 2-Bromo-5-(trifluoromethoxy)aniline belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

An aqueous solution of NaOH (10.2 g, 254 mmol in 20 mL water) was added to a solution of Preparation 67A in t-butanol (100 mL). Next, a solution of di- tert-butyldicarbonate (60.1 mL, 254 mmol) in t-butanol was added at room temperature and the resulting mixture was stirred for 4 days. The reaction mixture became a suspension and was filtered. The residue was washed with a small amount of water. The filtrate was concentrated to half its volume and then extracted with EtOAc (2 x 200 mL). The organic layer was washed with brine solution and dried over anhydrous Na2SO4. Removal of solvent in vacuo gave Preparation 67B (31.0 g) as a white solid.

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, 2-Bromo-5-(trifluoromethoxy)aniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; WO2009/3077; (2008); A1;,
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Adding a certain compound to certain chemical reactions, such as: 10075-63-5, name is 1,5-Dimethoxynaphthalene, belongs to ethers-buliding-blocks compound, 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 10075-63-5, Safety of 1,5-Dimethoxynaphthalene

General procedure: To [Ir(COD)OMe]2 (7.3 mg, 11 mumol) and 4,4′-di-tert-butyl-2,2′-bipyridine (7.0 mg, 26 mumol) in a flame-dried vial under nitrogen were added THF (0.7 mL), pinacolborane (0.18 mL, 1.24 mmol) and 1,4-dimethoxynaphthalene (7) (188 mg, 1.0 mmol). The mixture was stirred at 80 C for 24 h then filtered through Celite and concentrated in vacuo to afford crude pinacol ester 13 (100% conversion by 1H NMR) that was used directly in the next step.

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, 1,5-Dimethoxynaphthalene, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Hume, Paul; Furkert, Daniel P.; Brimble, Margaret A.; Tetrahedron Letters; vol. 53; 29; (2012); p. 3771 – 3773;,
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Adding a certain compound to certain chemical reactions, such as: 15799-79-8, name is 3-Methoxy-N,N-dimethylaniline, belongs to ethers-buliding-blocks compound, 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 15799-79-8, Formula: C9H13NO

[0086] (R)-3-(4-Dimethylamino-2-methoxy-phenyl)-butyraldehyde (Table 1, entry 1). To a 2-dram vial equipped with a magnetic stir bar was added (2S,5S)-5-benzyl-2-tert-butyl-3-methylimidazolidin-4-one (12.3 mg, 0.050 mmol, 0.100 equiv), CH2Cl2 (0.50 ml), HCl (as a 4N solution in 1,4-dioxane, 12.5 uL, 0.050 mmol, 0.100 equiv), and N,N-dimethyl-m-anisidine (73.3 uL, 0.500 mmol, 1.00 equiv). The solution was cooled to -40o C. before crotonaldehyde (124 uL, 1.50 mmol, 3.00 equiv) was added. After 36 h, the reaction mixture was subjected directly to silica gel chromatography. Elution with 20% EtOAc in hexanes followed by concentration and removal of residual crotonaldehyde under vacuum afforded the product as a colorless oil in 86% yield (94.9 mg, 0.429 mmol); 89% ee. IR (film) 2958, 2874, 2834, 2719, 1721, 1615, 1568, 1516, 1462, 1441, 1352, 1238, 1133, 1034, 979.6, 814.0 cm-1; 1H NMR (300 MHz, CDCl3) ?9.67 (t, J=2.7 Hz, 1H, CHO), 7.03 (d, J=8.2 Hz, 1H, ArH), 6.31 (dd, J=2.5, 8.2 Hz, 1H, ArH), 6.27 (d, J=2.5 Hz, 1H, ArH), 3.83 (s, 3H, OCH3), 3.63 (dq, J=7.1, 7.1 Hz, 1H, ArCH), 2.94 (s, 6H, N(CH3)2), 2.68 (ddd, J=2.5, 6.9, 15.9 Hz, 1H, CH2CO), 2.55 (ddd, J=2.8, 7.7, 15.9 Hz, 1H, CH2CO), 1.27 (d, 3H, CHCH3); 13C NMR (75 MHz, CDCl3) ?203.7, 157.8, 150.9, 127.5, 121.7, 15.1, 96.6, 55.4, 51.2, 41.0, 27.6, 20.9. HRMS (CI) exact mass calcd for (C13H19NO2) requires m/z 222.1494 for [M+H]+, found m/z 222.1497. [?]D=-9.5 (c=1.0, CHCl3). The enantiomeric ratio of the product was determined by HPLC analysis of the corresponding alcohol (obtained by NaBH4 reduction) using a Chiracel AD and AD guard column (3.0% ethanol/hexanes, 1 mL/min); S isomer tr=21.6 min, R isomer tr=23.1 min.

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.

Reference:
Patent; MacMillan, David W.C.; Paras, Nick A.; US2003/236438; (2003); A1;,
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Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 17600-72-5, name is 1-Ethoxy-2-methoxybenzene, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of 1-Ethoxy-2-methoxybenzene

A 2-way cock with a septum at the tip was attached to a recovery flask containing o-ethoxymethoxybenzene (150 mg, 0.98 mmol) and dried by allowing to stand overnight under reduced pressure in the presence of diphosphorus pentoxide, It was returned to atmospheric pressure with nitrogen. After reducing the pressure with a diaphragm pump again, hydrogen iodide gas (127 mg, 0.99 mmol) was introduced from the septum using a 50 mL syringe and returned to atmospheric pressure by filling with nitrogen and then allowed to stand at 25 C. for 48 hours I put it. After the reaction, the mixture was reduced in pressure by a diaphragm pump to obtain a mixture (139.0 mg) of o-ethoxyphenol, o-methoxyphenol and o-ethoxymethoxybenzene. The yield was determined to be 77%: 9%: 14% o-ethoxyphenol: o-methoxyphenol: o-ethoxymethoxybenzene from the integration ratio of 1 H-NMR using phenanthrene as an internal standard.

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 17600-72-5.

Reference:
Patent; Chiba University; Godo Shigen Co., Ltd; Matsumoto, Shoji; Akazome, Motohiro; Otani, Yasuhiko; (14 pag.)JP5725506; (2015); B2;,
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Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 121588-79-2, name is trans-4-Methoxycyclohexanamine, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: trans-4-Methoxycyclohexanamine

4.71 g (10 mmol) of compound VII was dissolved in 20 ml of 1,4-dioxane.Add to the solution1.937 g (15 mmol) of trans-4-methoxycyclohexylamine and 0.12 ml of glacial acetic acid,The mixture was heated to reflux for 15 hours, and the reaction mixture was concentrated under reduced pressure, and then evaporated,The solid was dispersed, suction filtered, and the filter cake was washed with 10 ml of ethanol and dried.Crude4.62g,The yield was 78.4%.

According to the analysis of related databases, 121588-79-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Beijing Concorde Pharmaceutical Er Factory; Chinese Academy Of Medical Sciences Pharmaceutical Institute; Zhang Dongfeng; Huang Haihong; Li Chun; Yin Dali; Lin Ziyun; Ma Chen; Wang Mijuan; Zhang Meng; Lan Pei; Zhao Limin; (11 pag.)CN109748903; (2019); A;,
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Adding a certain compound to certain chemical reactions, such as: 887267-47-2, name is 2-Bromo-5-(trifluoromethoxy)aniline, belongs to ethers-buliding-blocks compound, 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 887267-47-2, Computed Properties of C7H5BrF3NO

To a solution of 2-bromo-5-(trifluoromethoxy)benzenamine (1.0 g, 3.9 mmol) in 20 mL of tetrahydrofuran were added /V,//-dimethylpyridin-4-amine (50 mg, 0.4 mmol), and di-tert-butyl dicarbonate (2.55 g,11.7 mmol). The resulting mixture was stirred at reflux for overnight. After cooled to room temperature, the solvent was removed in vacuo and the residue was purified by silica gel column chromatography (petroleum ether: ethyl acetate = 10: 1) to give 1.4 g (80%) of the product as a white solid. MS (ESIpos): m/z = 456 (M+H)+; LC-MS [Method 2] : R, = 1.07 min.

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

Reference:
Patent; BAYER AKTIENGESELLSCHAFT; BAYER PHARMA AKTIENGESELLSCHAFT; NGUYEN, Duy; WORTMANN, Lars; FARIA ALVARES DE LEMOS, Adelaide, Clara; BOeMER, Ulf; SUeLZLE, Detlev; HOLTON, Simon; LECHNER, Christian; (147 pag.)WO2019/170543; (2019); A1;,
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Electric Literature of 887267-47-2, The chemical industry reduces the impact on the environment during synthesis 887267-47-2, name is 2-Bromo-5-(trifluoromethoxy)aniline, I believe this compound will play a more active role in future production and life.

The aryl halide (e.g., 1.00 mmol), triethylamine (e.g., 2.00 mmol) and P(o-tol)3 (e.g., 0.30 mmol) were dissolved in acetonitrile (e.g., 0.5 M) in a glass pressure tube and nitrogen gas was bubbled through the solution via a gas dispersion tube for 10 minutes. Ethyl acrylate (e.g., 1.25 mmol) and palladium acetate (e.g., 0.10 mmol) were added to the reaction mixture and the tube was sealed and placed into an oil bath pre-heated to about 120 0C for about 18 h. The resulting solution was concentrated under vacuum and purified (e.g., silica gel column).The title compound was prepared from 2-bromo-5-(trifluoromethoxy)aniline according to protocol M. Retention time (min) = 2.693, method [1], MS(ESI) 276.1 (M+Eta).

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, 2-Bromo-5-(trifluoromethoxy)aniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ELAN PHARMACEUTICALS, INC.; SHAM, Hing, L.; KONRADI, Andrei, W.; HOM, Roy, K.; PROBST, Gary, D.; BOWERS, Simeon; TRUONG, Anh; NEITZ, R., Jeffrey; SEALY, Jennifer; TOTH, Gergely; WO2010/91310; (2010); A1;,
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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. 456-55-3, name is (Trifluoromethoxy)benzene, A new synthetic method of this compound is introduced below., HPLC of Formula: C7H5F3O

EXAMPLE 2 4-Trifluoromethoxy-alpha,alpha,alpha-trifluoroacetophenone was prepared from 4-bronotrifluoromethoxybenzene by a procedure similar to that described in Example 1. 4-Bromotrifluoromethoxybenzene may be prepared from trifluoromethoxybenzene by the process described in the Journal of Organic Chemistry, 29, 1, (1964). Boiling point: 164-166 C. (atmosphere pressure). 1 H NMR (CDCl3)delta (ppm): 7.35, 8.14 (4H,d), 19 F NMR (CDCl3)delta (ppm relative to CFCl3): -58.1 (s) CF3 O. -72.1 (s) CF3.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; Imperial Chemical Industries PLC; US4891450; (1990); 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. 38603-09-7, name is 1,3-dibromo-2-methoxybenzene belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Quality Control of 1,3-dibromo-2-methoxybenzene

To a THF solution of 2,6-dibromoanisole (10 g, 37.6 mmol) was added Mg (0.90 g, 37.6 mmol), and the mixture was heated and stirred at 40C. Under ice-cooling, n-heptanal (47.2 g, 41.3 mmol) was added dropwise. Aqueous hydrochloric acid solution was added to the reaction mixture, this was extracted with ethyl acetate, and the solvent was distilled off to obtain 8.95 g of a compound (1). NMR (CDCl3) delta ppm: 7.45 – 7.48 (m, 1H), 7.35 – 7.38 (m ,1H), 7.01 (t, 1H, 8.1 Hz), 4.96 – 5.00 (m, 1H), 3.88 (s, 3H), 1.70 – 1.80 (m, 2H), 1.25 – 1.63 (m ,8H), 0.85 – 0.90 (m, 3H)

The synthetic route of 38603-09-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Shionogi&Co., Ltd.; EP2184279; (2010); A1;,
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