Author: tianli

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, 10488-69-4, blongs to alcohols-buliding-blocks compound. Formula: C6H11ClO3

Preparation of (S) 6-chloro-5~hydroxy-N,N-diisopropyl-3-oxo hexanamide(Formula-12a) N-N-diisopropylacetamide (70 grams) added to a solution of 3500 ml of 1 molarLiHMDS solution, 650 ml of tetrahydrofuran at -50 to -700C. Stirred the reaction mixture for 25 minutes at -70 to -750C. Added 185 gram of ethyl-4-chloro-3 -hydroxy butanoate at -73 to -75¡ãC. Stirred the reaction for 1 hour at -48 to -45¡ãC. Quenched the reaction mixture with chilled water followed by hydrochloric acid solution. Separated the organic and inorganic phases. Washed the organic layer with 10percent sodium bicarbonate solution. Dried the organic layer using sodium sulfate and distilled the solvent completely under reduced pressure. Purified the residue in petroleum ether to get the title compound of formula- 12. Yield: 240 grams

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,10488-69-4, its application will become more common.

Reference:
Patent; SATYANARAYANA REDDY, Manne; THIRUMALAI RAJAN, Srinivasan; SAHADEVA REDDY, Maramreddy; WO2008/44243; (2008); A2;,
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Electric Literature of 504-63-2, 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.504-63-2, name is 1,3-Propanediol, molecular formula is C3H8O2, molecular weight is 76.0944, as common compound, the synthetic route is as follows.

To a dried 250 mL RBF under an atmosphere of argon at room temperature was added 1 00 mL of distilled THF and 2.1 g of sodium hydride (60% dispersion in mineral oil; Aldrich). The mixture was stirred vigorously and 1 ,3-propanediol (4.0 g, 50 mmol; Aldrich) was added over 1 0 minutes via syringe. The reaction was allowed to stir for 45 minutes before tert-butyldimethylsilyl chloride (7.9 g, 52.7 mmol; Aldrich) was added portion wise over 5 minutes. The reaction was then allowed to stir for a further 45 minutes at room temperature before being quenched slowly with 20 mL of 10% aqueous sodium carbonate solution. This mixture was then transferred to a separatory funnel. After being vigorously shaken, the biphasic mixture was separated and the aqueous phase was further extracted with two 50 mL portions of ether. The combined organic phases are then dried with sodium sulfate and filtered through a plug of 1 inch of Celite and 1 inch of flash silica (silica gel 60, EMD) via a 100 mL sinter funnel under vacuum into a 500 mL RBF, with the sodium sulfate residue washed with a further 50 mL of ether. The collected solution was then reduced under vacuum on a Buchi rotary evaporator to give compound L, as a light yellow oil in 99% yield and >95% purity

Statistics shows that 504-63-2 is playing an increasingly important role. we look forward to future research findings about 1,3-Propanediol.

Reference:
Patent; THE FLORIDA STATE UNIVERSITY RESEARCH FOUNDATION; PREVACUS, INC.; CRAN, John, W.; HAN, Yinglin; ZHANG, Faliang; WO2014/145302; (2014); A2;,
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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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Related Products of 124-68-5, 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 124-68-5, name is 2-Amino-2-methyl-1-propanol. This compound has unique chemical properties. The synthetic route is as follows.

A 2 L Morton flask equipped with overhead stirring was charged with dichloromethane (200 ml_), 2-amino-2-methylpropan-1-ol (10.71 ml_, 112 mmol) and a saturated solution of sodium bicarbonate (200 ml_) and the reaction mixture was stirred. Benzyl chloroformate (16.61 ml_, 1 18 mmol) was added rapidly via syringe to the reaction mixture and stirring was continued (1H NMR after 6 hours indicated complete conversion). The mixture was poured into a separatory funnel and the layers were separated. The organic layer was washed with water and saturated sodium chloride, dried over sodium sulfate, and concentrated in vacuo to afford a colorless liquid (23.5 g). This liquid was purified by silica gel chromatography, eluting with ethyl acetate: heptane (1 :9 to 1 :1) to afford benzyl (1-hydroxy-2-methylpropan-2-yl)carbamate (13.61 g, 61.0 mmol, 54.3 % yield) as a colorless syrup. NMR (400 MHz, CD3SOCD3) d 1 .16 (s, 6 H), 3.35 (d, J = 6 Hz, 2 H), 4.69 (t, J = 6 Hz, 1 H), 4.97 (s, 2 H), 6.69 (br s, 1 H), 7.26-7.42 (m, 5 H); LC-MS (LC-ES) M+H = 224.

According to the analysis of related databases, 124-68-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; GLAXOSMITHKLINE INTELLECTUAL PROPERTY DEVELOPMENT LIMITED; CADILLA, Rodolfo; DEATON, David Norman; LARKIN, Andrew L; SCHULTE, Christie; SMALLEY JR, Terrence L.; (237 pag.)WO2020/95215; (2020); 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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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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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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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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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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Application of 1124-63-6, 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. 1124-63-6, name is 3-Cyclohexylpropan-1-ol. A new synthetic method of this compound is introduced below.

F. 0.2 g of the catalyst prepared in Example 1, 14.2 mg (0.1 mmol) 3-cyclohexyl-1-propanol and 10 mg dodecane as an internal standard were added to 5 ml of 5 mmol (0.43 g) pivalaldehyde in xylene, and the mixture was allowed to react for 4.5 hours under reflux. The product was analyzed by gas chromatography and GC-MS. As a result, the product was identified as 3-cyclohexylpropyl aldehyde. Gas chromatography analysis indicated 45 % yield.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,1124-63-6, 3-Cyclohexylpropan-1-ol, and friends who are interested can also refer to it.

Reference:
Patent; JAPAN TOBACCO INC.; EP603409; (1994); A1;,
Alcohol – Wikipedia,
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