Month: June 2021

Synthetic Route of 16545-68-9, 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 16545-68-9 as follows.

[000296j Compounds 5-bromo-2-fluoropyridine (25.0 g, 0.12 mol) and cyclopropanol (02, 10.4 g, 0.18 mol) were dissolved in NMP (100 mL) and treated with potassium tertbutoxide (180 mL, lMsolution in THF, 0.18 mol) at 0 C. The solution became dark and cloudy, and warmed. After 30 mm, the reaction mixture was partitioned between ethyl acetate and petroleum ether (500 mL, 1/1 v/v) and water (500 mL). The organic layer was separated, washed with water and 5% aq. LiC1, dried over anhydrous sodium sulfate, filtered and concentrated. The residue was purified with silica gel column chromatography (ethyl acetate in petroleum ether, 10% v/v) to furnish Compound 03. ?H-NMR (CDC13, 400 MHz) major characteristic peaks: (5(ppm) 0.74-0.81 (m, 4H), 4.13-4.18 (m, 1H), 6.88 (d, J= 8.8 Hz, 1H), 7.66 (dd, J 8.8, 2.4 Hz, 1H), 8.26 (d, J 2.4 Hz, 1H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,16545-68-9, its application will become more common.

Reference:
Patent; BIOMARIN PHARMACEUTICAL INC.; WANG, Bing; WO2015/65937; (2015); A1;,
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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.

Step -1: Synthesis of Compound 2: TBSCI ^ 0C-rt, 30 min <, [0094] Alcohol (8,92 mmol) was added into a round bottom flask followed by OT (36 rriL) and cooled to 0 (. Imidazole ( 1 .04 mmol) was added and allowed to stir for 5 minutes. FBSCi (8,92 mmol) was added in portion wise and continued the stirring for 30 min. The reaction was quenched with 20 niL water. Organic layer was separated and dried over anhydrous ajSO* Concentration in vacuo and purification by flash column chromatography gave silyi ether 2. 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 110-73-6, 2-(Ethylamino)ethanol. Reference:
Patent; KANDULA, Mahesh; WO2013/168023; (2013); A1;,
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Electric Literature of 454-91-1, 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 454-91-1, name is 1-[3-(Trifluoromethyl)phenyl]ethanol. This compound has unique chemical properties. The synthetic route is as follows.

Example 87 1-[3-(Trifluoromethyl)phenyl]ethyl N-{4-[(6,7-dimethoxy-4-quinolyl)oxy]phenyl}carbamate 4-[(6,7-Dimethoxy-4-quinolyl)oxy]aniline (74 mg) was added to toluene/triethylamine = 10/1 (7 ml), and the mixture was heated under reflux to prepare a solution. A solution of triphosgene (115 mg) in methylene chloride was then added to the solution, and the mixture was heated under reflux for 15 min.Subsequently, 3-trifluoromethyl-alpha-methylbenzyl alcohol (70 mg) was added thereto, and the mixture was further stirred with heating under reflux for 2 hr. After the completion of the reaction, the reaction solution was allowed to cool to room temperature before distilled water was added thereto. The mixture was subjected to separatory extraction with chloroform, followed by washing with a 1 N aqueous hydrochloric acid solution and saturated brine. The washed solution was dried over sodium sulfate and was concentrated. The residue was purified on a column using chloroform/methanol to give the title compound (81 mg, yield 59%). 1H-NMR (CDCl3, 400 MHz): 8.41 – 8.48 (1H, m), 8.11 (1H, s), 7.45 – 7.68 (7H, m), 7.13 – 7.18 (2H, m), 6.93 (1H, s), 6.65 (1H, d, J = 6.6 Hz), 5.94 (1H, q, J = 6.6 Hz), 4.14 (3H, s), 4.08 (3H, s), 1.63 (3H, d, J = 6.6 Hz) Mass spectrometry value (ESI-MS, m/z): 513 (M++1)

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 454-91-1, 1-[3-(Trifluoromethyl)phenyl]ethanol.

Reference:
Patent; KIRIN BEER KABUSHIKI KAISHA; EP1243582; (2002); A1;,
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Adding a certain compound to certain chemical reactions, such as: 5299-60-5, Ethyl 6-hydroxyhexanoate, 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: Ethyl 6-hydroxyhexanoate, blongs to alcohols-buliding-blocks compound. Recommanded Product: Ethyl 6-hydroxyhexanoate

Example 1 : Preparation of tetranor-PGDMPreparation of Ester (2A) from 6-hydroxyhexanoate (1A EtO.OTBDMSO2A(2, wherein R is ethylR2 is methyl, andR3 is ieri-butyl)- 50.0 g (312.1 mmol) of ethyl 6-hydroxyhexanoate (1A)- 61.15 g (405.72 mmol) of TBDMSC1;- 42.5 g (624.2) of imidazole;- 500 ml of DMF.[0048] A solution of ethyl 6-hydroxyhexanoate (1 A) in dry DMF was cooled with an ice bath and treated with TBDMSC1 and imidazole portion wise for 10 minutes. The cooling bath was removed and the reaction mixture was stin-ed overnight (controlled by TLC, hexane – ethyl acetate 90: 10). The next day the reaction mixture was treated with ice (200 g), stirred for 5 minutes, and extracted with H-EA (10: 1 , 800 ml, 2×200 ml). The combined organic phases were washed with water-brine (1 : 1 , 2 x 100 ml), brine (100 ml), dried over Na2SC>4, and evaporated. The residue was purified by flash chromatography: Silica gel (300 g), hexane (H) – ethyl acetate (EA) 100: 1 – 70: 1. The mass of the collected product (Ester (2 A)) was 81.5 g (95%), TLC Rf = 0.8 (solvent system: hexane – ethyl acetate 90: 10).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,5299-60-5, Ethyl 6-hydroxyhexanoate, and friends who are interested can also refer to it.

Reference:
Patent; CAYMAN CHEMICAL COMPANY, INCORPORATED; ENDRES, Gregory, W.; KORNILOV, Andriy, M.; UZIEBLO, Adam; WO2011/159740; (2011); A2;,
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Electric Literature of 27129-87-9, 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 27129-87-9 as follows.

Step 2: 3,5-Dimethylbenzyl 4-((tert-butoxycarbonyl)amino)piperidine-1-carboxylate To a stirred solution of (3,5-dimethylphenyl)methanol (1.020 g, 7.49 mmol) in DMF (5 mL) at RT was added CU (1.214 g, 7.49 mmol). The reaction mixture was heated at 50 C. for 20 hrs. Tert-butyl piperidin-4-ylcarbamate (1.5 g, 7.49 mmol) was added and the reaction mixture stirred at 50 C. for 4 hrs. The mixture was diluted with EtOAc and washed with a saturated solution of sodium bicarbonate, brine, dried over MgSO4, filtered and concentrated under reduced pressure. Purification was carried out by chromatography on silica using 0-100% EtOAc in hexanes as eluent to afford the title product. LC-M: Rt 1.47 mins; MS m/z 263.3, 264.2; [M-Boc]+; Method 2minLowpHv03

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,27129-87-9, its application will become more common.

Reference:
Patent; Novartis AG; Legrand, Darren Mark; Furminger, Vikki; Thomson, Christopher; Hughes, Owen Rhys; Stanley, Emily; US2014/171403; (2014); A1;,
Alcohol – Wikipedia,
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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. 13330-96-6, name is 4-(Dimethylamino)butan-1-ol, the common compound, a new synthetic route is introduced below. name: 4-(Dimethylamino)butan-1-ol

General procedure: 12 (100 mg, 0.35 mmol) was dissolved in the mixture of 1,4-dioxane (10 mL) and H2O (2.00 mL) and then added with boronicacid (2.80 mmol), Pd(dppf)2Cl2 (28 mg, 0.035 mmol) and Cs2CO3(228 mg, 0.70 mmol). The reaction was heated at 100 C underargon atmosphere. After 12 h, the reaction mixture was cooled toroom temperature and was concentrated in vacuo. Then themixture was diluted with water and extracted with ethyl acetate.The combined organic layer was washed by saturated sodiumchloride solution for three times, dried over anhydrous Na2SO4 andconcentrated under reduced pressure. The residue was purified bysilica gel chromatography to give 13.To a stirred solution of 13 and triphosgene (100 mg, 0.34 mmol)in anhydrous dichloromethane (5 mL) was added triethylamine(104 mg, 1.02 mmol) at 0 C under nitrogen atmosphere. After5 min, a solution of 4-(dimethylamino)butan-1-ol (1.02 mmol) indichloromethane (5.00 mL) was added and then the mixture wasstirred at room temperature for overnight. The reactionwas dilutedwith dichloromethane (15 mL) and washed with water (3 20 mL).The organic phases were dried over anhydrous Na2SO4 andconcentrated in vacuo. The residue was purified by using columnchromatography to afford the corresponding product.

The synthetic route of 13330-96-6 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Lu, Dong; Liu, Jianan; Zhang, Yunzhe; Liu, Feifei; Zeng, Limin; Peng, Runze; Yang, Li; Ying, Huazhou; Tang, Wei; Chen, Wuhong; Zuo, Jianping; Tong, Xiankun; Liu, Tao; Hu, Youhong; European Journal of Medicinal Chemistry; vol. 145; (2018); p. 328 – 337;,
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Electric Literature of 14593-04-5, 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. 14593-04-5, name is 3-Amino-3-phenyl-1-propanol, molecular formula is C9H13NO, 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 4-Chloro-2-[(3-Hydroxy-1-Phenylpropyl)Amino]-Benzonitrile A mixture of 3-amino-3-phenyl-1-propanol (1 g, 6.6 mmol), 4-chloro-2-fluorobenzonitrile (1 g, 6.4 mmol) and N,N-diisopropylethylamine (1.2 ml, 6.9 mmol) was stirred and heated at 140° C. for 5 h. The crude reaction mixture was cooled and purified on silica gel (ether/isohexane 1:4). The product was isolated as a colourless solid (1.1 g, 58percent), m.p. 88-90° C. MS APCI+vem/z287 ([M+H]+). 1H NMR 300 MHz (d6-DMSO) 7.5-7.2 (6H, m), 7.05 (1H, d), 6.63 (1H, dd), 6.51 (1H, d), 4.9 (1H, t), 4.73 (1H, q), 3.49 (2H, q), 2.1-1.88 (2H, m).

According to the analysis of related databases, 14593-04-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Cheshire, David; Connolly, Stephen; Cox, David; Millichip, Ian; US2003/73685; (2003); 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. 202865-66-5, name is (2-Bromo-5-fluorophenyl)methanol, the common compound, a new synthetic route is introduced below. Formula: C7H6BrFO

[2-Amino-6-[4-fluoro-2-(hydroxymethyl)phenyl]quinazolin-4-yl]isoindolin-2-ylmethanone (?A4?) [0341] 74 mg of (2-bromo-5-fluorophenyl)methanol, 100 mg of potassium carbonate, 1 ml of water and 15 mg of [1,1?-bis(diphenylphosphino)ferrocene]palladium(II) dichloride are added to a solution of 150 mg of [2-amino-6-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)quinazolin-4-yl]-(1,3-dihydroisoindol-2-yl)methanone in 3 ml of ethanol under argon. The mixture is heated at 120° C. for min; the hot mixture is filtered through kieselguhr, and the filtrate is evaporated in vacuo. The residue is purified by reverse-phase column chromatography. [0342] Yield: 8 mg (5percent) of [2-amino-6-[4-fluoro-2-(hydroxymethyl)phenyl]quinazolin-4-yl]isoindolin-2-ylmethanone; HPLC retention time: 1.51 min; [0343] 1H NMR (400 MHz, DMSO-d6/TFA-d1) delta [ppm] 8.08-8.02 (m, 2H), 7.81 (d, J=8.7, 1H), 7.42 (d, J=7.2, 1H), 7.39-7.25 (m, 4H), 7.24 (d, J=6.9, 1H), 7.16 (td, J=8.5, 2.8, 1H), 4.99 (s, 2H), 4.82 (s, 2H), 4.36 (s, 2H).

The synthetic route of 202865-66-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; MERCK PATENT GESELLSCHAFT MIT BESCHRANKTER HAFTUNG; Eggenweiler, Hans-Michael; Sirrenberg, Christian; Buchstaller, Hans-Peter; US2013/178443; (2013); A1;,
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Adding a certain compound to certain chemical reactions, such as: 623-61-0, Isopropyl glycolate, 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, 623-61-0, blongs to alcohols-buliding-blocks compound. Recommanded Product: 623-61-0

To the obtained isopropyl hydroxyacetate, 85.79 g of 99.5% sodium isopropoxide was added, and the alcohol formed by the reaction was removed at 50 C, and 212.60 g of 99% 1,2,3-trichlorobenzene was added thereto. The condensation reaction is carried out at 110 C,After the reaction, the unreacted 1,2,3-trichlorobenzene was removed under reduced pressure.The condensation liquid is cooled to 45 C for filtration, and the filter cake is dried under reduced pressure.The dried fractions are collected and combined with the filtrate.264.21g of isopropyl 2,3-dichlorophenoxyacetate, the content of 98.5%,The yield was 98.9%.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,623-61-0, its application will become more common.

Reference:
Patent; Shandong Runbo Biological Technology Co., Ltd.; Sun Guoqing; Chi Zhilong; Hou Yongsheng; Zhang Liguo; Hu Yishan; (8 pag.)CN108947816; (2018); A;,
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Adding a certain compound to certain chemical reactions, such as: 868594-48-3, 1-Phenyl-2,5,8,11,14,17,20,23,26-nonaoxaoctacosan-28-ol, 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: 868594-48-3, blongs to alcohols-buliding-blocks compound. Recommanded Product: 868594-48-3

Compound d (0.684 g, 1.36 mmol, 2 eq) and triethylene glycol dimethanesulfonate (0.208 g, 0.68 mmol, 1 eq),Sodium hydroxide (116 mg, 2.9 mmol, 4.3eq) was added to a round flask, dissolved in 5 ml of tetrahydrofuran, stirred at room temperature for 12 hours, and then distilled under reduced pressure to dry the solvent.Thereafter, 87 mg of a palladium / carbon catalyst (Palladium on carbon) was added thereto, dissolved in 35 ml of ethanol, and stirred with hydrogen gas at room temperature for 12 hours.After distillation under reduced pressure, the solvent was dried and dichloromethane / methanol 9: 1 was purified by silica gel normal chromatography with a developing solution to obtain pure Compound A-2 (0.300 g, 39.3%)

At the same time, in my other blogs, there are other synthetic methods of this type of compound,868594-48-3, 1-Phenyl-2,5,8,11,14,17,20,23,26-nonaoxaoctacosan-28-ol, and friends who are interested can also refer to it.

Reference:
Patent; Bio Aekcheu Co., Ltd.; Park Jin-u; Jang Su-jeong; Lee Bong-gyu; Yoon Hyeong-jun; Song Mi-yeong; (13 pag.)KR102027694; (2019); B1;,
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