Tag: M.W=100-200

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. 112-27-6, name is 2,2′-(Ethane-1,2-diylbis(oxy))diethanol. This compound has unique chemical properties. The synthetic route is as follows. category: alcohols-buliding-blocks

Under nitrogen, was added 200mL pyridine 1000ml three-neck flask,120 g BP103a00 (1.0 eq), stirred and cooled to 0 C, 151.8 g of TsCl (1.0 eq) was added in portions, and stirred for 1 h.Then slowly warm to room temperature and continue to stir for 3-4 h.After the reaction is completed, the reaction solution is poured into a dilute hydrochloric acid solution of ice, extracted with EA, and the EA layer is washed once with dilute hydrochloric acid. Washed with saturated sodium bicarbonate, washed with brine, dried over anhydrous Na2SO4, solvent was distilled off under reduced pressure, silica gel column chromatography to give pure BP103a01 55g

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, 112-27-6, 2,2′-(Ethane-1,2-diylbis(oxy))diethanol.

Reference:
Patent; Borui Bio-pharmaceutical (Suzhou) Co., Ltd.; Yuan Jiandong; Huang Yangqing; Song Yunsong; (20 pag.)CN109771658; (2019); 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.7314-44-5, name is (2,4-Dimethoxyphenyl)methanol, molecular formula is C9H12O3, molecular weight is 168.19, as common compound, the synthetic route is as follows.Recommanded Product: (2,4-Dimethoxyphenyl)methanol

N-(Fmoc)-M1-(Boc)-D-Tryptophan (1 eq., 4.5 g, 8.55 mmol), TBTU (1 eq., 2.74 g, 8.55 mmol) and di-iso-propylethylamine (DIEA, 2 eq., 2.82 mL, 17.1 mmol) were dissolved in DMF (20 mL), stirred at rt for 30 mm under argon atmosphere, treated with an injection of a solutionof 2,4-dimethoxybenzyl alcohol (1.1 eq., 1.58 g, 9.4 mmol, prepared according to Feng, L.; Lv, K.; Liu, M.; Wang, S.; Zhao, J.; You, X.; Li, S.; Cao, J.; Guo, H. Eur. J. Med. Chem. 2012, 55, 125-136) in DMF (5 mL), and stirred at rt for 4h. The reaction mixture was diluted with EtOAc and washed with water (2 x 100 mL) and brine (2 x 100 mL). The organic phases were combined, dried over Na2SO4, filtered and evaporated to a residue that was purified by flashchromatography on silica gel eluting with 20% EtOAc in hexane to afford ester 6 (4.97 g, 7.35 mmol, 86 %) as white solid: mp 67-68 C; Rf 0.29 (20% EtOAc in hexane); 1H NMR (500 MHz, CDCI3) oe 8.11 (brs, 1H), 7.76 (d, J= 7.6 Hz, 2H), 7.58-7.48 (m, 3H), 7.44 (s, 1H), 7.42-7.36 (m, 2H), 7.33 – 7.26 (m, 3H), 7.21 (t, J 7.3 Hz, 1 H), 7.11 (d, J = 8.0 Hz, 1 H), 6.46 – 6.39 (m, 2H), 5.44 (d, J= 8.0 Hz, 1H), 5.12 (s, 2H), 4.78 (dd, J= 13.6, 5.4 Hz, 1H), 4.40-4.28 (m, 2H),4.19 (t, J= 7.3 Hz, 1H), 3.80 (s, 3H), 3.79 (s, 3H), 3.33-3.20 (m, 2H), 1.65 (s, 9H); 13C NMR(125 MHz, CDCI3) 6 171.7, 161.7, 159.2, 155.8, 149.7, 144.0, 143.9, 141.4 (2C), 131.7 (2C),127.8 (2C), 127.2 (2C), 125.3 (2C), 124.6 (2C), 124.5, 124.4, 122.8, 120.1, 119.0, 115.8, 115.4,115.1, 104.2, 98.7, 83.8, 67.3, 63.4, 55.5 (2C), 54.4, 47.3, 28.3 (3C), 28.0; HRMS m/zcalculated for C40H41N208 [M+H] 677.2857; found 677.2859.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,7314-44-5, (2,4-Dimethoxyphenyl)methanol, and friends who are interested can also refer to it.

Reference:
Patent; VALORISATION-RECHERCHE, LIMITED PARTNERSHIP; LUBELL, William D.; ONG, Huy; ZHANG, Jinqiang; MULUMBA, Dilan Mukandila; MARLEAU, Sylvie; OHM, Ragnhild Gaard; AHSANULLAH, -; OMRI, Samy; CHINGLE, Ramesh; (157 pag.)WO2018/79; (2018); A1;,
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Application of 37585-16-3, 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. 37585-16-3, name is (2-Amino-4-chlorophenyl)methanol. A new synthetic method of this compound is introduced below.

General procedure: To a solution of but-2-ynoic acid (8 mmol, 1 equiv) and 2-aminobenzylalcohol (8 mmol, 1 equiv) in CH2Cl2 (60 mL) at 0 C was added a solution of N,N?-dicyclohexylcarbodiimide (DCC) (8 mmol, 1 equiv) in CH2Cl2 (20 mL) dropwise. The mixture was stirred at room temperature overnight, and then filtrated through a short pad of celite. The filtrate was concentrated and used for the next step without further purication. The crude solid was added to a suspension of pyridinium chlorochromate (PCC) (1.5-2.0equiv) and celite in CH2Cl2 (80 mL). The mixture was stirred at room temperature for 1-4 h, then filtrated and puried by silica gel column chromatography to give the product. The above crude solid was dissolved in THF (50 mL) and was added to a solution of NaH (1.3 equiv.) in THF (20 mL) dropwise at 0 C. The mixture was stirred at 0 C for half an hour, then MeI (1.3 equiv.) was added. The reaction mixture was stirred at room temperature until completion as monitored by TLC and then quenched by addition of saturated aqueous NH4Cl solution. The mixture was extracted with EtOAc, and the organic layer was washed with H2O and brine, dried over anhydrous Na2SO4, filtered, and concentrated under vacuum. The residue was puried by column chromatography on silica gel (eluent: ethyl acetate/petroleum ether = 1/4) to afford products 1b-1g.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,37585-16-3, its application will become more common.

Reference:
Article; Zhang, Xiaojuan; Han, Xiuling; Chen, Junjie; Lu, Xiyan; Tetrahedron; vol. 73; 12; (2017); p. 1541 – 1550;,
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Electric Literature of 14002-80-3, 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. 14002-80-3, name is Methyl 3-hydroxy-2,2-dimethylpropanoate, molecular formula is C6H12O3, 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 solution of methyl 3-hydroxy-2,2-dimethylpropanoate (5.00 g, 38 mmol), N, N-diisopropylethylamine (7.30 g, 57 mmol) and tert- butyldimethylchlorosilane (6.80 g, 45 mmol) in dry DMF (70 mL) was stirred at room temperature for 12 h. The reaction solution was quenched with water (225 mL) and extracted with diethyl ether (3 x 50 mL). The combined organic extracts were washed with water (100 mL), brine (100 mL), then dried over MgSO4. Concentration under reduced pressure afforded methyl 3-(tert-butyldimethylsilyloxy)-2,2- dimethylpropanoate as colorless oil (9.36 g, 100%). It was used in the next step without further purification. 1H NMR (300 MHz, CDCl3) delta 3.64 (s, 3H), 3.55 (s, 2H), 1.13 (s, 6H), 0.85 (s, 9H), 0.0 (s, 6H).

According to the analysis of related databases, 14002-80-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; AMBIT BIOSCIENCE CORPORATION; APUY, Julius, L.; INSKI, Darren, E.; JAMES, Joyce, K.; WO2010/54058; (2010); 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.44565-27-7, name is 4-Amino-2-methylbutan-1-ol, molecular formula is C5H13NO, molecular weight is 103.1628, as common compound, the synthetic route is as follows.name: 4-Amino-2-methylbutan-1-ol

Reference Example 39 tert-Butyl (4-{[tert-butyl(dimethyl)silyl]oxy}-3-methylbutyl)carbamate A solution of di-tert-butyl dicarbonate (11.1 g) in methylene chloride (30 mL) was added to a solution of 4-amino-2-methylbutan-1-ol (5.00 g) in methylene chloride (50 mL) with stirring at room temperature. After stirring overnight at room temperature, the reaction solution was washed with a saturated aqueous solution of ammonium chloride, a saturated aqueous solution of sodium bicarbonate, and saturated sodium chloride solution in this order. The organic layer was dried over anhydrous sodium sulfate, then filtered, and concentrated under reduced pressure. The obtained residue was dissolved in methylene chloride (150 mL). To the solution, tert-butyldimethylchlorosilane (8.77 g) and imidazole (8.25 g) were added with stirring at 0 C. The mixture was heated to room temperature and stirred overnight, and the reaction solution was then washed with water, a 1 M aqueous citric acid solution, and saturated sodium chloride solution in this order. The organic layer was dried over anhydrous sodium sulfate, then filtered, and concentrated under reduced pressure to obtain the title compound (16.2 g). 1H-NMR (CDCl3) delta: 0.04 (6H, s), 0.89 (3H, d, J=6.6 Hz), 0.89 (9H, s), 1.27-1.38 (1H, m), 1.44 (9H, s), 1.53-1.70 (2H, m), 3.07-3.15 (1H, m), 3.17-3.25 (1H, m), 3.39-3.47 (2H, m), 4.70 (1H, br s).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,44565-27-7, 4-Amino-2-methylbutan-1-ol, and friends who are interested can also refer to it.

Reference:
Patent; DAIICHI SANKYO COMPANY, LIMITED; Nagata, Tsutomu; Kobayashi, Jun; Onishi, Yoshiyuki; Kishida, Masamichi; Noguchi, Kengo; US2013/12532; (2013); A1;,
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Adding a certain compound to certain chemical reactions, such as: 117284-59-0, 2-(2,2-Difluorocyclopropyl)ethanol, 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: 117284-59-0, blongs to alcohols-buliding-blocks compound. Recommanded Product: 117284-59-0

At 0C, to a solution of Cr03 (5.70 g, 57.00mmol) in sulfuric acid (8.3 mL) was added water (92 mL). Then a solution of 2-(2,2- difluorocyclopropyl)ethan-1-ol (180 mg, 1.47 mmol) in acetone (30 mL) was added dropwise over 20 mm period. The resulting mixture was stirred for 4 h at room temperature. Whe the reaction was done, the reaction mixture was extracted with ether (50 mL x 4). The organic layers were combined, washed with 2 M sodium hydroxide solution (50 mL x 4) and the aqueous layers were combined. The pH value of the resulting aqueous solution was adJusted to 1 using sulfuric acid and extracted with ether (50 mL x 4). The organic phases were combined, washed with brine and dried over Na2SO4. The solvent was removed under reduced pressure to yield 2-(2,2- difluorocyclopropyl)acetic acid as colorless oil (117 mg, 58%). GCMS: m/z = 136 [Mj.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,117284-59-0, 2-(2,2-Difluorocyclopropyl)ethanol, and friends who are interested can also refer to it.

Reference:
Patent; MERCK PATENT GMBH; SHERER, Brian A.; BRUGGER, Nadia; (546 pag.)WO2017/106607; (2017); A1;,
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Electric Literature of 148043-73-6, 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 148043-73-6 as follows.

To an aqueous solution of pentafluoropentanol (1M, 1.0 g, 5.61 mmol) was addedtetraethylammonium hydrogen sulfate (10.21mg, 0.045 mmol). The solution was heated to 70 C and an aqueous solution of sodium permanganate monohydrate (1.5M, 1.257 g, 7.86 mmol) was added over 20 minutes. The reaction was stirred at 70 C for an additional 4 hours. The reaction mixture was filtered through Celite (diatomaceous earth). The filter cake was washed with hot water (10 mL). The aqueous solution was acidified to a pH = 1 with concentrated sulfuric acid (200 uL) and extracted with methyl tert-butyl ether (3 10 mL). The organic fractions were combined and dried over magnesium sulfate, filtered and concentrated. NMR (500 MHz, CH3 CN-ds ): delta 2.59 (t, J = 7.5 Hz, 2H); 2.49-2.39 (m, 3H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,148043-73-6, its application will become more common.

Reference:
Patent; MERCK SHARP & DOHME CORP.; RAGHAVAN, Subharekha; STELMACH, John, E.; SMITH, Cameron, J.; LI, Hong; WHITEHEAD, Alan; WADDELL, Sherman, T.; CHEN, Yi-Heng; MIAO, Shouwu; ORNOSKI, Olga, A.; GARFUNKLE, Joie; LIAO, Xibin; CHANG, Jiang; HAN, Xiaoqing; GUO, Jian; GROEPER, Jonathan, A.; BROCKUNIER, Linda, L.; ROSAUER, Keith; PARMEE, Emma, R.; WO2011/149921; (2011); 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. 597-31-9, name is 3-Hydroxy-2,2-dimethylpropanal. This compound has unique chemical properties. The synthetic route is as follows. Application In Synthesis of 3-Hydroxy-2,2-dimethylpropanal

Hydrogenation; The starting solution used was the mixture described above as hydrogenation feed. From 0 to 7% by weight (based on the hydrogenation feed) of a 15% by weight aqueous solution of trimethylamine (from 2 to 5% by weight (based on the hydrogenation feed), or of a 5% by weight aqueous solution of citric acid in the comparative examples) were added to this mixture in order to establish the particular pH of the hydrogenation effluent specified in Table 1. The hydrogenation feed thus obtained was pumped over the catalyst in a hydrogenation reactor with liquid circulation (circulation:feed=10:1) with a catalyst hourly space velocity of 0.4 kgHPA/Icat¡Áh in trickle mode at 40 bar and 120 C.A comparison of the process according to the invention with comparative examples V1 and V2, in which the pH of the hydrogenation effluent is in each case outside the inventive range, is shown by Table 1.For pH measurement, a Knick model 766 pH meter with a Schott N1041A glass electrode was used.

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, 597-31-9, 3-Hydroxy-2,2-dimethylpropanal.

Reference:
Patent; BASF SE; US2009/69604; (2009); 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. 10029-04-6, name is Ethyl 2-(hydroxymethyl)acrylate. A new synthetic method of this compound is introduced below., name: Ethyl 2-(hydroxymethyl)acrylate

General procedure: To a solution of the appropriate allylic alcohol 6 (1.00 equiv.) in dichloromethane (0.1 M) was added vinyl acetic acid 7 (1.20 equiv.), dicyclohexylcarbodiimide (1.20 equiv.) and 4-N,N-dimethylaminopyridine (0.15 equiv.) at 0C. The mixture was allowed to warm to ambient temperature and stirred until the product was fully converted (TLC). The solution was filtered and the filter cake was washed three times with dichloromethane. The combined organic layers were washed with aq. HCl (1 M) and then with saturated aq. NaHCO3 solution, dried with Na2SO4, filtered and dry-loaded on silica gel. The pure product was obtained after column chromatography on silica, using hexane/MTBE mixtures of increasing polarity as eluents.

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, 10029-04-6, Ethyl 2-(hydroxymethyl)acrylate.

Reference:
Article; Schmidt, Bernd; Audoersch, Stephan; Kunz, Oliver; Synthesis; vol. 48; 24; (2016); p. 4509 – 4518;,
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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. 2240-88-2, name is 3,3,3-Trifluoropropan-1-ol, molecular formula is C3H5F3O, 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. Formula: C3H5F3O

Intermediate 31 3f3-trifluoropropoxy)methyl)pyrimidine To a solution of (2-chloro-6-(l-ethoxyvinyl)pyrimidin-4-yl)methyl methanesulfonate (0.452 g, 1.54 mmol) in benzene (7 mL) were added 3,3,3-trifluoropropan-l-ol (0.264 g, 2.32 mmol), sodium hydroxide (5 M, 0.463 mL, 2.32 mmol) and tetrabutylammonium hydrogen sulfate (0.052 g, 0.15 mmol). The mixture was stirred vigourously over night at room temperature. The mixture was filtered through a short silica plug with magnesium sulfate on top. The filter was washed with EtOAc. The mixture was purified by preparative HPLC to give 2-chloro-4-(l- ethoxyvinyl)-6-((3,3,3-trifluoropropoxy)methyl)pyrimidine 0.055 g 11 percent). MS (ES+) m/z 311 [M+H]+.

With the rapid development of chemical substances, we look forward to future research findings about 2240-88-2.

Reference:
Patent; ACTURUM LIFE SCIENCE AB; BESIDSKI, Yevgeni; YNGVE, Ulrika; PAULSEN, Kim; LINDE, Christian; MACSARI, Istvan; MALMBORG, Jonas; PAPTCHIKHINE, Alexander; ARVIDSSON, Per; WO2014/195323; (2014); A1;,
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