Month: June 2021

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. 28539-02-8, name is 1-(Hydroxymethyl)benzotriazole. A new synthetic method of this compound is introduced below., Formula: C7H7N3O

To a solution of 3 ,4,6-trimethyl-2-(5 -((1 -methylcyclopropyl)methoxy)-2-azabicyclo[4. 1. Ojheptan-2-yl)-6,7-dihydro-5H-pyrrolo[3,4-bjpyridin-5-one (77 mg, 0.217 mmol) in THF (1 mL) was added LiHMDS (1.083 ml, 1.083 mmol) at -78C. Then the mixture was stirred at -78 C for 30 mm. Then(1H-benzo[dj[1,2,3jtriazol-1-yl)methanol (48.5 mg, 0.325 mmol) in THF (1 mL) was dropwise added to the mixture and the mixture was stirred for another 30 mm. The reaction mixture was diluted with water (10 mL) and extracted with EtOAc (10 mLx 2). The combined organic layers were dried over Na2504 and filtered, and the filtrate was concentrated in vacuo to give the residue, which was further purified by prep-TLC (dichloromethane : MeOH = 10:1) to provide the title compound as yellow oil. The title compound was separated by chiral SFC (AD(250mm*3Omm,lOum), 30% MeOH with 0.1%NH3.H20/C02 at 6OmL/min) and Prep-HPLC (TFA) to give four isomers. Example 5 (firstpeak): MS: 386.1 (M+1). ?H NMR (400 MHz, Methanol-d4): oe 4.23-4.25 (1 H, m), 4.11-4.14 (2H, m), 3.97-3.99 (1 H, m), 3.79-3.82 (1 H, m), 3.46-3.49 (1 H, m), 3.33-3.35 (1 H, m), 3.13 (3H, s), 2.94-3.01 (2 H, m), 2.60 (3 H, s), 2.36 (3 H, s), 1.95-2.01 (1 H, m), 1.46-1.70 (2 H, m),1.14 (3 H, s), 0.87-0.92 (1 H, m), 0.58-0.61 (1 H, m), 0.42-0.45 (2 H, m), 0.30-0.32 (2 H, m).Example 6 (second peak): MS: 386.2 (M+1). ?H NMR (400 MHz, Methanol-d4): oe 4.23-4.25 (1H, m), 4.11-4.14 (2 H, m), 4.01-4.04 (1 H, m), 3.79-3.82 (1 H, m), 3.46-3.49 (1 H, m), 3.32-3.35(1 H, m), 3.13 (3 H, s), 2.94-3.01 (2 H, m), 2.60 (3 H, s), 2.36 (3 H, s), 1.95-2.01 (1 H, m), 1.46-1.70 (2 H, m), 1.14 (3 H, s), 0.87-0.92 (1 H,m), 0.58-0.61 (1 H, m), 0.42-0.45 (2 H, m), 0.30-0.32 (2 H, m). Example 7 (third peak): MS: 386.2 (M+1). ?H NMR (400 MHz, Methanol-d4): oe4.23-4.25(1 H, m), 4.11-4.14(2 H, m), 4.01-4.02 (1 H, m), 3.79-3.82 (1 H, m), 3.45-3.47(1 H,m), 3.32-3.35 (1 H, m), 3.13 (3 H, s), 2.94-3.01 (2 H, m), 2.60 (3 H, s), 2.36 (3 H, s), 1.95-2.01(1 H, m), 1.46-1.70 (2 H, m), 1.14 (3 H, s), 0.87-0.92 (1 H, m), 0.58-0.61 (1 H, m), 0.42-0.45 (2H, m), 0.3 1-0.32 (2 H, m). Example 8 (fourth peak): MS: 386.1 (M+1).?H NMR (400 MHz,Methanol-d4): oe 4.23-4.26(1 H, m), 4.11-4.14(2 H, m), 3.98-4.01 (1 H, m), 3.79-3.82(1 H, m), 3.45-3.47 (1 H, m), 3.32-3.35 (1 H, m), 3.13 (3 H, s), 2.94-3.01 (2 H, m), 2.60 (3 H, s), 2.36 (3 H, s), 1.95-2.01 (1 H, m), 1.46-1.70 (2 H, m), 1.14 (3 H, s), 0.87-0.92 (1 H, m), 0.58-0.61 (1 H, m), 0.42-0.44 (2 H, m), 0.3 1-0.32 (2 H, m).

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, 28539-02-8, 1-(Hydroxymethyl)benzotriazole.

Reference:
Patent; MERCK SHARP & DOHME CORP.; CLAUSEN, Dane James; FELLS, James, I.; KOZLOWSKI, Joseph, A.; LIU, Ping; MAZZOLA, Robert, D., Jr.; (94 pag.)WO2018/226545; (2018); A1;,
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Adding a certain compound to certain chemical reactions, such as: 124-68-5, 2-Amino-2-methyl-1-propanol, 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: 124-68-5, blongs to alcohols-buliding-blocks compound. Recommanded Product: 124-68-5

2-Amino-2-methyl-l-propanol (5 g, 56.1 mmol), (Boc)20 (13.46 g, 61.7 mmol) and triethyl amine (6.24 g, 61.7 mmol) were dissolved in 50 mL of dichloromethane. The reaction mixture was stirred for 4 h at 22 to 25 C. Above mixture was washed with water (25 mL x 2), dried over anhydrous sodium sulfate and concentrated under vacuum to get tert-buty] (1- hydroxy-2-methylpropan-2-yl)carbamate (10.3 g, 97% yield).

The synthetic route of 124-68-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; NEKTAR THERAPEUTICS (INDIA) PVT.LTD.; NEKTAR THERAPEUTICS (Incorporated under the Laws of Delaware and domiclled in the State of California); DUARTE, FRANCO; ANAND, NEEL; SHARMA, PANKAJ; SINGH, DEVENDRAPRATAP U.; WO2015/79459; (2015); A1;,
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Electric Literature of 10488-69-4, 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. 10488-69-4, name is Ethyl 4-chloro-3-hydroxybutanoate, molecular formula is C6H11ClO3, 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.

Take raw materialsS-4-chloro-3-hydroxybutyric acid ethyl ester 5 g,Add a bottle of bottles,Add 10 ml of methanol,Add 5 g of sodium azide to stir,The reaction was carried out at a temperature of about 50 ° C for 4 hours to stop the reaction to obtain a yellow solution.20 ml of water was added, and the mixture was extracted with 20 ml of ethyl acetate, and the ethyl acetate was concentrated to obtain a yellow oil as an intermediate.

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 10488-69-4, Ethyl 4-chloro-3-hydroxybutanoate.

Reference:
Patent; Chongqing Runze Pharmaceutical Co., Ltd.; Ye Lei; (12 pag.)CN107011235; (2017); A;,
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Related Products of 15258-73-8, 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 15258-73-8 as follows.

2,6-Dichlorobenzyl alcohol (1.1 mmol) was dissolved in dry DMF (5 ml) and treated with sodium hydride (60% dispersion in mineral oil, 1.21 mmol). The mixture was stirred at room temperature for 30 mins, then treated with lithium-5-chloro-pyrazine-2- carboxylate (1 mmol) and stirred at reflux overnight. The reaction mixture was partitioned between ethyl acetate and water, then the organic layer was separated, dried [(MGSO4),] filtered, evaporated and the residue purified by column chromatography on silica. Elution with mixtures of petroleum ether and diethyl ether afforded the title product. MS (ES): m/e 300 (M+H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,15258-73-8, its application will become more common.

Reference:
Patent; ASTEX TECHNOLOGY LIMITED; WO2004/4720; (2004); A1;,
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Application of 395-23-3, Adding some certain compound to certain chemical reactions, such as: 395-23-3, name is Phenyl(4-(trifluoromethyl)phenyl)methanol,molecular formula is C14H11F3O, 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 395-23-3.

General procedure: Caution. tert-Butyl hydroperoxide is an exceptionally dangerous chemical that is highly reactive, flammable, and toxic. It is corrosive to skin and mucous membranes and causes respiratory distress when inhaled. A solution of secondary alcohol (1 mmol) and 70% TBHP (6 or 10 equiv.) was stirred at 100 C for 24 h. The reaction mixture was quenched with the saturated solution of sodium thiosulfate (5 mL) and extracted with dichloromethane (3 x 10 mL). The combined dichloromethane extracts were dried over anhydrous Na2SO4 and filtered, and then the solvent was removed under reduced pressure. The residue was purified by flash column chromatography on silica gel with PE or PE/EtOAc as the eluent to obtain the desired products.

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. 395-23-3, Phenyl(4-(trifluoromethyl)phenyl)methanol, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Wu, Jianglong; Liu, Yan; Ma, Xiaowei; Liu, Ping; Gu, Chengzhi; Dai, Bin; Synthetic Communications; vol. 46; 21; (2016); p. 1747 – 1758;,
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Related Products of 14002-80-3, 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 14002-80-3 as follows.

Intermediate 5: Methyl 2,2-dimethyl-3-oxopropanoateTo a solution of methyl 3-hydroxy-2,2-dimethylpropanoate (2 g, 15.13 mmol) and TEMPO (0.236 g, 1.513 mmol) in dichloromethane (15 ml) was added iodobenzene diacetate (5.36 g, 16.65 mmol) and the solution was stirred for 3 hours at ROOM TEMPERATURE. The reaction was quenched with a saturated solution of NaHCtheta3/5%Na2S2theta3 (10ml) and extracted with DCM (20ml). The organic layer was washed with brine and then dried (Na2SO4), filtered and evaporated to afford the title compound (4.8 g, 14.75 mmol) as an -1 :1 mixture with iodobenzene that was used in the following reaction without further purification; 1H NMR (CDCI3) only signals relating to title compound: delta 1.38 (s, 6H), 3.78 (s, 3H), 9.69 (s, 1 H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,14002-80-3, its application will become more common.

Reference:
Patent; GLAXO GROUP LIMITED; DI FABIO, Romano; GIANOTTI, Massimo; LESLIE, Colin Philip; STASI, Luigi Piero; WO2010/142652; (2010); A1;,
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Electric Literature of 517-21-5, 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. 517-21-5, name is Sodium 1,2-dihydroxyethane-1,2-disulfonate. A new synthetic method of this compound is introduced below.

General procedure: To a solution of the corresponding compound 3 (0.9 mmol) in ethanol/water (30 mL/4 mL) was added glyoxal sodium bisulfite hydrate (975 mg, 15 mmol) and the resulting suspension was stirred at 100C overnight. The solvent was removed in vacuo and the residue was partitioned between water and EtOAc. The organic layer was separated and washed with water and brine, dried over Na2S04 and concentrated, purified by flash column to give title product 4, which was confirmed by LCMS.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,517-21-5, Sodium 1,2-dihydroxyethane-1,2-disulfonate, and friends who are interested can also refer to it.

Reference:
Patent; AGIOS PHARMACEUTICALS, INC.; POPOVICI-MULLER, Janeta; ZAHLER, Robert; YE, Zhixiong; WO2014/139144; (2014); A1;,
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Electric Literature of 6351-10-6, 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. 6351-10-6, name is 2,3-Dihydro-1H-inden-1-ol. A new synthetic method of this compound is introduced below.

General procedure: A mixture of alcohol (0.5 mmol) in the case of solids, which had been powedered for 1-2 min and halosilanes (0.55 mmol) was transferred to a 4 mL screw-capped vial, and stirred at rt or heated at 70-75 C for 0.5 h-24 h. The progress of the reaction mixture was monitored by TLC. Upon completion of the reaction, the crude reaction mixture was cooled down to the room temperature and volatile product (TMS)2O was removed by evaporation at 30-35oC under reduced pressure and the remaining was analysed by 1H NMR. Finally, if necessary, the pure final product was obtained after column chromatography on dried silica. Detailed experimental information such as isolated yields, and spectroscopic and other identification data are given in Characterization Data of Isolated Final Products chapter in the SI.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,6351-10-6, its application will become more common.

Reference:
Article; Ajvazi, Njomza; Stavber, Stojan; Tetrahedron Letters; vol. 57; 22; (2016); p. 2430 – 2433;,
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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. 1805-32-9, name is 3,4-Dichlorobenzyl alcohol. This compound has unique chemical properties. The synthetic route is as follows. Recommanded Product: 1805-32-9

General procedure: The alcohol (1 mmol) was added to a mixture of TBHP(1 mmol) and VO(ephedrine)2MNPs (50 mg) in PEG(1 mL), and then the mixture was refluxed at 80 C for thetime specified. The progress was monitored by TLC (EtOAc/n-hexane, 1/2). After completion of the reaction, the catalystwas separated from the product by an external magnet(within 5 s), and the mixture was washed with EtOAc(25 mL) and decanted. The decanted mixturewas washedwith 30% NaOH (5 mL) and the organic layer was dried overanhydrous Na2SO4. The evaporation of EtOAc underreduced pressure gave the pure products in 85e98% yields.

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, 1805-32-9, 3,4-Dichlorobenzyl alcohol.

Reference:
Article; Rostami, Amin; Pourshiani, Omid; Darvishi, Neda; Atashkar, Bahareh; Comptes Rendus Chimie; vol. 20; 4; (2017); p. 435 – 439;,
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Electric Literature of 7073-69-0, 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 7073-69-0 as follows.

INTERMEDIATE 15; ferf-Butyl-4- { [2-(2-fluoropropan-2-yl)phenyl] carbonyl } piperidine- 1 -carboxylate; Step 1 : l-Bromo-2-(2-fluoropropan-2-yl)benzene; Into a 100 mL round-bottom flask equipped with a magnetic stir bar was dissolved 2-(2-bromophenyl)propan-2-ol (1.0 g, 4.7 mmol) in CH2Cl2 (15 mL) and it was cooled to -78 C. DAST (1.1 g, 7.0 mmol) was added and the reaction was monitored by TLC. After disappearance of the starting material, the reaction mixture was quenched over 50 mL of a sat aq. NaHCO3 solution in a beaker. It was then transferred into a 250 mL separatory funnel and extracted with ethyl acetate (2 x 70 mL). Combined organic layers were washed with brine, dried over MgSO4, filtered and the solvent was evaporated under reduced pressure. Purification by column chromatography through silica gel, eluting with 100% hexanes afforded the title compound.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,7073-69-0, its application will become more common.

Reference:
Patent; MERCK FROSST CANADA LTD.; ISABEL, Elise; LACHANCE, Nicolas; LECLERC, Jean-Philippe; LEGER, Serge; OBALLA, Renata, M.; POWELL, David; RAMTOHUL, Yeeman, K.; ROY, Patrick; TRANMER, Geoffrey, K.; ASPIOTIS, Renee; LI, Lianhai; MARTINS, Evelyn; WO2010/94126; (2010); A1;,
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