Month: June 2021

Adding a certain compound to certain chemical reactions, such as: 92093-23-7, 1-(4-Bromophenyl)ethane-1,2-diol, 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, Safety of 1-(4-Bromophenyl)ethane-1,2-diol, blongs to alcohols-buliding-blocks compound. Safety of 1-(4-Bromophenyl)ethane-1,2-diol

Alternative preparation of chiral 71rans-Lambda/-[2-(4-bromophenyl)cyclopropyl]-2- propanesulfonamide Enantiomer 1 and Enantiomer 2 EPO enantiomer 2enantiomer 1 Intermediate 7 Intermediate 7 enantiomer 2 Enantiomer 1 Enantiomer 2 trans trans; Intermediate 9, Enantiomer 1: chiral 2-(4-bromophenyl)oxirane Enantiomer 1; A 50OmL round bottom flask, equipped with magnetic stirrer, was charged with 10OmL of 1BuOH, 10OmL of water and of AD-mix-beta(30.6g). Stirring at room temperature produced two clear phases; the lower aqueous one appeared bright yellow. The mixture was cooled to 00C whereupon some of the dissolved salts precipitated. 4-Br-styrene (4g, 21.85mmol) was added at once and the heterogeneous slurry was stirred vigorously at 00C for 3h. While the mixture was stirred at 00C, solid sodium sulfite (32.8g) was added and the mixture was allowed to warm to room temperature and stirred for 1h. 20OmL DCM was added to the reaction mixture and after separation of the layers the aqueous one was further extracted with DCM (3x10OmL). Combined organic extracts were dried over Na2SO4 and evaporated to dryness to get 4.9g of crude material as a colourless thick oil.3.9g of this oil (17.97mmol) were dissolved in dry DCM 5OmL, under nitrogen. To this solution trimethylorthacetate (2.962mL, 23.27mmol) was added and the mixture cooled down to O0C. TMS-CI (2.964mL, 23.36mmol) was added dropwise and the reaction mixture left reacting for 1.5h. The volatiles were evaporated and the residue was dissolved in MeOH, treated with K2CO3 (3.1 g) and stirred vigorously at room temperature for 3h. The suspension was filtered, the solid was washed with DCM and the filtrate was evaporated in a rotary evaporator at room temperature under EPO vacuum to get crude title material (3.9g) that was purified by SiO2 flash chromatography eluting with petroleum ether/Et2O from 95/5 to 90/10. Evaporation of the solvent afforded title material, 2.95g, as a colourless oil that became a waxy solid in the fridge. NMR (CDCI3): 7.49 (d,2H), 7.13 (d, 2H), 3.84 (dd, 1 H), 3.13 (dd, 1 H), 2.77 (dd, 1 H). Chiral HPLC: ee 98.6% Analytical Chiral HPLC conditions: column: CHIRALPAK AS-H (25×0.46 cm) mobile phase: n-Hexane/Ethanol 95/5% v/v flow rate: 1 ml/minUV wavelength range: 200-400 nm Rt Enantiomer 1 : 6.1 min 99.3 a/a% Rt Enantiomer 2: 8.5min 0.7 a/a%.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,92093-23-7, 1-(4-Bromophenyl)ethane-1,2-diol, and friends who are interested can also refer to it.

Reference:
Patent; GLAXO GROUP LIMITED; WO2006/87169; (2006); A1;,
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Related Products of 946122-05-0, 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 946122-05-0, name is (2-Amino-4-bromophenyl)methanol. This compound has unique chemical properties. The synthetic route is as follows.

Acetophenone (144 mg, 1.2 mmol),[Cp * Ir (6,6 ‘- (OH) 2bpy) (H2O)] [OTf] 2 (8.3mg, 0.01mmol, 1mol%), potassium hydroxide (56mg, 1.0mmol, 1.0 equiv.),2-Amino-4-bromobenzyl alcohol (201 mg, 1.0 mmol) and water (1 mL) were sequentially added to a 5 mL round bottom flask. After the reaction mixture was refluxed in air for 12 hours,Cool to room temperature. It was extracted with ethyl acetate, the solvent was removed by rotary evaporation and then purified by column chromatography (developing solvent: petroleum ether / acetic acidEthyl ester) to give the pure target compound in a yield of 94%

While traditionally a conservative industry, chemical producers will need to modernize their PR strategies to stay relevant.we look forward to future research findings about 946122-05-0, (2-Amino-4-bromophenyl)methanol.

Reference:
Patent; Nanjing University of Science and Technology; Li Feng; Wang Rongzhou; (15 pag.)CN107400084; (2017); A;,
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Related Products of 110-73-6, 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 110-73-6, name is 2-(Ethylamino)ethanol. This compound has unique chemical properties. The synthetic route is as follows.

Synthesis of(Intermediate 3) 60ml of N, N-dimethylacetamide Intermediate 2 was added 21.1 g(50 mmol), and stirred in an ice bath, was added dropwise so as to keep the following 10 C N- ethyl ethanolamine 8.9 g (100 mmol) . After completion ofthe dropwise addition, stirring under an ice bath for 2 hours, ethyl acetate100ml reaction solution, ion-exchanged water 100ml, and extracted concentratedhydrochloric acid was added to 3 ml. The organic layer was washed with asaturated sodium chloride aqueous solution, dried over anhydrous magnesiumsulfate, and the solvent was evaporated. Then purified by silica gel columnchromatography (hexane / ethyl acetate = 1/1), Intermediate 3 19.0 g: yield(yield: 80%).

According to the analysis of related databases, 110-73-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; FUJIFILM Corporation; Takasaki, Yuta; Ishiwata, Yasuhiro; Morozumi, Kazuma; (58 pag.)JP2015/124376; (2015); A;,
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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.623-69-8, name is 1,3-Dimethoxypropan-2-ol, molecular formula is C5H12O3, molecular weight is 120.15, as common compound, the synthetic route is as follows.name: 1,3-Dimethoxypropan-2-ol

To a solution of 1, 3-dimethoxy-2-hydroxypropane (3.84g, 0. 032mol) in DCM (70ml) cooled at 5 C was added triethylamine (Sml, 0. 036mol) followed by slow addition of methanesulphonyl chloride (2. 72ml, 0. 035mol). The mixture was then stirred at ambient temperature for 24 hours. The mixture was then absorbed onto silica gel and purified by flash silica chromatography DCM: isohexane (3: 1) to give the title compound (3.74g, 59percent). NMR 3.15 (s, 3H), 3.28 (s, 6H), 3.52 (d, 4H), 4.78 (q, 1H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,623-69-8, 1,3-Dimethoxypropan-2-ol, and friends who are interested can also refer to it.

Reference:
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; WO2003/76436; (2003); A1;,
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Synthetic Route of 756520-66-8, 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 756520-66-8, name is 1-(2,6-Dichloro-3-fluorophenyl)ethanol. This compound has unique chemical properties. The synthetic route is as follows.

2. To a stirred solution of triphenyl phosphine (8.2 g, 0.03 mol) and DEAD (13.65 mL of a 40% solution in toluene) in THF (200 mL) at 0C was added a solution of 1-(2,6- dichloro-3-fluoro-phenyl)-ethanol (4.55 g, 0.021 mol) and 3-hydroxy-nitropyridine (3.35 g, 0.023 mol) in THF (200 mL). The resulting bright orange solution was stirred under a nitrogen atmosphere at ambient temperature for 4 hours at which point all starting materials had been consumed. The solvent was removed, and the crude material was dry loaded onto silica gel, and eluted with ethyl acetate-hexanes (20:80) to yield 3-(2,6- dichloro-3-fluoro-benzyloxy)-2-nitro-pyridine (6.21 g, 0.02 1 mol, 98%) as a pink solid. 1H NMR (CDCI3, 300 MHz) 61.8-1.85 (d, 3H), 6.0-6.15 (q, 1H), 7.0-7.1 (t, 1H), 7.2-7.21 (d, 1H), 7.25-7.5 (m, 2H), 8.0-8.05 (d, 1H).

While traditionally a conservative industry, chemical producers will need to modernize their PR strategies to stay relevant.we look forward to future research findings about 756520-66-8, 1-(2,6-Dichloro-3-fluorophenyl)ethanol.

Reference:
Patent; PFIZER INC.; CHRISTENSEN, James Gail; ZOU, Yahong; WO2013/17989; (2013); A1;,
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Reference of 7218-43-1, 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. 7218-43-1, name is 2-[2-(2-Propynyloxy)ethoxy]ethanol. A new synthetic method of this compound is introduced below.

A suspension of Intermediate B (190 mg, 0.297 mmol), 2-(2-(prop-2-yn-1-yloxy)ethoxy) ethanol [King-Underwood et al., WO2011/048111] (257 mg, 0.890 mmol), PdCI2(PPh3)2 (208 mg, 0.297 mmol) and copper(l) iodide (57 mg, 0.30 mmol) in a mixture of Et2NH and DMF (4: 1 v/v, 7.5 ml_) was degassed with N2 and was then heated to 60C for 16 hr. The reaction mixture was cooled to RT and was evaporated in vacuo onto silica gel and purified by flash column chromatography (Si02, 12 g, MeOH in DCM, 0-5%, gradient elution) to afford the title compound, Compound (la), as a pale tan solid (30 mg, 14%); Rt 1.88 min, m/z 704 (M+H)+ (ES+); 1 H NMR delta: 3.36-3.50 (6H, overlapping m), 3.61-3.63 (2H, overlapping m), 4.37 (2H, s), 4.58 (1 H, m), 5.48 (2H, s), 5.76 (2H, s), 6.41 (1 H, d), 6.64 (1 H, m), 6.72 (1 H, d), 6.78 (1 H, s), 7.14 (1 H, t), 7.27 (1 H, t), 7.52 (1 H, d), 7.65-7.71 (2H, overlapping m), 7.82 (1 H, t), 8.13 (1 H, s), 10.19 (1 H, br s).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,7218-43-1, its application will become more common.

Reference:
Patent; RESPIVERT LIMITED; ONIONS, Stuart Thomas; COPMANS, Alex Herman; BROECKX, Rudy Laurent Maria; SMITH, Alun John; TADDEI, David Michel Adrien; WO2014/140597; (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.2240-88-2, name is 3,3,3-Trifluoropropan-1-ol, molecular formula is C3H5F3O, molecular weight is 114.07, as common compound, the synthetic route is as follows.Application In Synthesis of 3,3,3-Trifluoropropan-1-ol

To a solution of 3,3,3-trifluoropropan-1-ol (5.0 g, 43.8 mmol) in CH2Cl2 (25 mL) and pyridine (25 mL) was added 4-(dimethylamino)pyridine (0.27 g, 2.2 mmol) followed by p-toluenesulfonyl chloride (8.4 g, 43.8 mmol). The mixture was allowed to stir at ambient temperature for 72 h then was quenched with 5percent aqueous HCl (20 mL). The layers were separated and the aqueous phase was extracted with CH2Cl2 (3.x.7 mL). The combined organic extracts were dried over Na2SO4, filtered, and concentrated under reduced pressure. Purification by column chromatography (SiO2, 75percent hexanes in EtOAc) afforded the title compound (8.0 g, 29.8 mmol, 68percent yield). MS (DCI/NH3) m/z 286 (M+NH4)+

At the same time, in my other blogs, there are other synthetic methods of this type of compound,2240-88-2, 3,3,3-Trifluoropropan-1-ol, and friends who are interested can also refer to it.

Reference:
Patent; ABBOTT LABORATORIES; US2010/69348; (2010); A1;,
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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. 2425-41-4, name is (2-Phenyl-1,3-dioxane-5,5-diyl)dimethanol, the common compound, a new synthetic route is introduced below. Application In Synthesis of (2-Phenyl-1,3-dioxane-5,5-diyl)dimethanol

Example 1A; 5,5′-Bis(octyloxymethyl)-2-phenyl-1 ,3-dioxane (1 a); 1a[00105] Sodium hydride (60% oil dispersion, washed with hexanes, 8.6 g, 0.22 mol, 2.0 5 eq) is added in portions slowly to a stirred solution of mono-O-benzylidenepentaerythritol (II, Scheme 1 , prepared by the method of Issidorides, C. H.; Gulen, R. C. Organic Syntheses Collected Volume IV, Rabjohn, N., Ed.; John Wiley and Sons: New York, 1963; pp 679-681) (24.11 g, 0.1076 mol) in dry DMF (600 ml_) under a nitrogen atmosphere. The stirred reaction mixture is cooled with an ice water bath for one hour,10 then 1-bromooctane (46.76 ml_, 51.90 g, 0.268 mol, 2.5 eq) is added dropwise over 2 h. After the reaction mixture has been stirred 12 h, another addition of sodium hydride (4.5 g, 0.11 mol, 1.0 eq) and 1-bromooctane (20 ml_, 0.11 mol, 1.0 eq) is made. If after the reaction mixture has been stirred a further 12 h, TLC shows that some mono-O-octyl product is present, another identical addition is made. When all of the mono-O-octyl15 derivative has been consumed, the reaction mixture is quenched by the addition of methanol dropwise until foaming ceases. The reaction mixture is filtered under vacuum and the reaction flask and filter are washed with dichloromethane (~150 ml_). The combined filtrate and washings are concentrated and the residue is extracted with hexanes (300 mL, then 200 ml_). The combined extracts are washed with water (10020 mL), dried (MgSO4) and concentrated under reduced pressure to an oily residue that is passed through a short silica gel column using hexanes, then 5% ethyl acetate/95% hexanes as eluents. The title compound (1a) is a colourless oil (44.71 g, 93 %): RF 0.46 (94 : 6, hexanes : ethyl acetate); 1H NMR (500.13 MHz) delta 0.88, 0.89 (2 t, 6H, J = 6.5 Hz, 2 x Me), 1.20-1.35 (br m, 2OH, 10 x CH2), 1.54, 1.57 (2 pentet, 4H, J = 6.8 Hz, 225 OCH2CH2), 3.22 (s, 2H, eq CCH2O), 3.35 (t, 2H, J = 6.5 Hz, eq octyl OCH2), 3.45 (t, 2H, J = 6.6 Hz, ax octyl OCH2), 3.71 (s, 2H, ax OCH2C), 3.88, 4.09 (2d, 4H, J = 11.5 Hz, H- 4,H-4′, H-6.H-6′), 5.42 (s, 1 H, acetal H), 7.31-7.49 (m, 5H, Ph); 13C NMR delta 138.5 (q Ph) , 128.8 (para Ph), 128.3 (2C, mPh), 126.1 (2C, oPh), 101.7 (acetal C), 71.8 (eq OCH2CH2), 71.7 (ax OCH2CH2), 70.8 (eq OCH2C), 70.2 (C-4 and C-6), 69.4 (ax OCH2C),30 38.9 (q C), 2 x 31.89 (CH2CH2CH3), 29.68, 29.54, 29.51 , 29.45, 2 x 29.34 (6 octyl CH2), 26.22, 26.19 (CH2CH2CH2O), 2 x 22.70 (CH2CH3), 14.3 (Me); MS ESI: CaIc for C28H49O4 449.3631 , found 449.2; calc for C28H48O4Na+ 471.35, found 471.3; calc for (C28H68O4)2Ca2+ 468.34, found 468.5; calc for C28H48O4K+ 487.32, found 487.3.

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

Reference:
Patent; ST. FRANCIS XAVIER UNIVERSITY; MARANGONI, D. Gerrard; GRINDLEY, T. Bruce; JAHAN, Nusrat; PETROPOLIS, Christian; TRAN, Thomas; PAUL, Nawal; WO2010/48715; (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. 5333-42-6, name is 2-octyldodecan-1-ol. A new synthetic method of this compound is introduced below., category: alcohols-buliding-blocks

2-octyldecanol (2-Octyldecanol) (4.3 g, 14.5 mmol)Anhydrous DMFIt was dissolved in0 In NaH (60% dispersion inparaffin) (0.58 g, 14.5 mmol) to It was added. After stirring 1 hour the reaction solution at 0 With 5,6-difluoro-benzo [c] [1,2,5] – thiadiazole was added (1 g, 5.8 mmol). Then, and after stirring at room temperature for 12 hours to terminate the reaction was added to a saturated NH4Cl solution and extracted with 100 mL of diethyl ether.The extract solution after silica gel column chromatography was concentrated by vacuum distillation (DCM: Hexanes (1: 3)) to give the compound through a 1 (4.0 g, 95% yield).

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, 5333-42-6, 2-octyldodecan-1-ol.

Reference:
Patent; Korea Research Institute of Chemical Technology; Lee, Jong Chul; Mun, Sang Jin; Sin, Won Suk; Lee, Sang Gyu; Song, Chang Uhn; Soh, Won Wook; Woo, Han Young; (18 pag.)KR2016/31958; (2016); A;,
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Reference of 7073-69-0, 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.7073-69-0, name is 2-(2-Bromophenyl)propan-2-ol, molecular formula is C9H11BrO, molecular weight is 215.087, as common compound, the synthetic route is as follows.

In a 250 mL three-necked flask, 0.03 mol of dibenzofuran-2-amine, 0.04 mol, was added under nitrogen.2-(2-Bromophenyl)propan-2-ol, 150 mL of toluene was stirred and mixed, then 0.05 mol of sodium t-butoxide, 0.0015 mol of Pd2 (dba) 3, 0.0015 mol of tri-tert-butylphosphine, and heated to 115 C, Reflow reaction for 24 hours; naturally cool to room temperature, filter, filterThe liquid was subjected to vacuum distillation (-0.09 MPa, 85 C), and passed through a neutral silica gel column to obtain2-(2-(dibenzo[b,d]furan-2-ylamino)phenyl)propan-2-ol

The chemical industry reduces the impact on the environment during synthesis 7073-69-0, I believe this compound will play a more active role in future production and life.

Reference:
Patent; Jiangsu March Optoelectric Technology Co., Ltd.; Miao Kangjian; Zhang Zhaochao; Zhang Xiaoqing; Li Chong; (43 pag.)CN108164470; (2018); A;,
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