Author: tianli

Adding a certain compound to certain chemical reactions, such as: 35106-82-2, (2-Vinylphenyl)methanol, 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, 35106-82-2, blongs to alcohols-buliding-blocks compound. name: (2-Vinylphenyl)methanol

Step 3: (1,3-dihydroisobenzofuran-1-yl)methanol To a mixture of (2-vinylphenyl)methanol (obtained from step 2) (1.0 g, 7.45 mmol) in DCM (10 mL) was added m-CPBA (1.82 g, 8.94 mmol) in small portions at 0¡ã C. The reaction mixture was stirred at room temperature for overnight, and then the mixture was diluted with DCM (30 mL) and washed with saturated NaHCO3 aqueous solution and brine. The organic layer was dried over sodium sulfate and concentrated under vacuum. The residue was purified by prep-TLC (petroleum ether:ethyl acetate=4:1) to afford (1,3-dihydroisobenzofuran-1-yl) methanol (260 mg, yield: 23percent) as yellow oil. m/z: [M+H]+ 151.1

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,35106-82-2, its application will become more common.

Reference:
Patent; SHANGHAI DE NOVO PHARMATECH CO. LTD.; GAO, Daxin; YANG, Heping; WANG, Pei; (84 pag.)US2017/37038; (2017); A1;,
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Application of 3840-31-1, Adding some certain compound to certain chemical reactions, such as: 3840-31-1, name is (3,4,5-Trimethoxyphenyl)methanol,molecular formula is C10H14O4, 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 3840-31-1.

Commercial available (3,4,5-trimethoxyphenyl)methanol (25 g, 126 mmol) was dissolved in THF (150 mL). Sodium hydride (3.93 g, 164 mmol) was added portionwise at 0C. The reaction mixture was stirred at 0C for 10 min. Then iodomethane (10.21 ml, 164 mmol) was added drop wise. The resultant mixture was stirred from 0C to rt for 3 hours and quenched by pouring into ice. The mixture was extracted with ethyl acetate, washed by brine and dried by anhydrous sodium sulfate. After filtered and concentrated, the afforded residue was purified by silica gel column. Colorless oil l,2,3-trimethoxy-5-(methoxymethyl)benzene (26.44 g, 125 mmol, 99 % yield) was afforded. 1H NMR (400 MHz, CDC13) delta 6.53 (s, 2H), 4.35 (s, 2H), 3.82 (s, 6H), 3.79 (s, 3H), 3.36 (s, 3H). 13C NMR (101 MHz, CDC13) delta 153.22 (2C), 137.36, 133.82, 104.53 (2C), 74.83, 60.76, 58.11, 56.02 (2C). ESI-MS m/z: 235.0 (MNa+).

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. 3840-31-1, (3,4,5-Trimethoxyphenyl)methanol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; THE UNITED STATES OF AMERICA, represented by THE SECRETARY, DEPARTMENT OF HEALTH & HUMAN SERVICES; ZHAO, Xue, Zhi; HUGHES, Stephen, H.; VU, Bao-Han, Christie; SMITH, Steven; JOHNSON, Barry; POMMIER, Yves; BURKE, Terrence, R., Jr.; WO2013/16441; (2013); A1;,
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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. 311-86-4, name is 2-Bromo-3,3,3-trifluoropropan-1-ol, molecular formula is C3H4BrF3O, 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. Recommanded Product: 2-Bromo-3,3,3-trifluoropropan-1-ol

2-bromo-1 ,1 , 1-trifluoropropan-3-ol (10 g, 0.0524mol) was placed in a 2-necked round bottom flask fitted with a distillation set up and then heated to 95 C. Sodium hydroxide (3 g, 0.0754 mol) was dissolved in water (12 g) at 0 C with stirring. Once the solution was homogenous it was then added dropwise to the 2-bromo-1 ,1 , 1-trifluoropropan-3-ol with rapid stirring via dropping funnel. As the head temperature reached 60 C clear liquid was collected in a receiver flask (4.2 g). GC area%: 1 , 1 , 1-trifluoro-1 ,2- epoxypropane (52%), 2-bromo-3,3,3-trifluoropropene + ethyl ether (26%), 3-acetoxy-2- bromo-1 , 1 , 1-trifluoropropane (7%), acetone (2%), unknown (13%).

With the rapid development of chemical substances, we look forward to future research findings about 311-86-4.

Reference:
Patent; MEXICHEM FLUOR S.A. DE C.V.; MURRAY, James Henry; SHARRATT, Andrew Paul; (32 pag.)WO2018/197897; (2018); A1;,
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Synthetic Route of 702-82-9 ,Some common heterocyclic compound, 702-82-9, molecular formula is C10H17NO, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route.

General procedure: To a suspension of 3a (206 mg, 0.748 mmol) in DMF (10 mL) was added DIPEA (0.392 mL, 2.245 mmol) and the solution was stirred at rt for 30 min. HBTU (568 mg, 1.497 mmol) was added portion wise, followed by the addition of 1-aminoadamantane (0.136 g, 0.898 mmol). The mixture was stirred at rt for 4 h and diluted with EtOAc (60 mL), washed with water (3 x 10 mL), HCl (0.5 M, 10 mL), water (10 mL) and brine (15 mL). Solvents were removed under reduced pressure and the residue was purified with flash chromatography using hexane:EtOAc (10:1 to 2:1) to give RS-005 (263 mg, 0.644 mmol, 86% yield).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,702-82-9, its application will become more common.

Reference:
Article; Slavik, Roger; Herde, Adrienne Mueller; Bieri, Daniel; Weber, Markus; Schibli, Roger; Kraemer, Stefanie D.; Ametamey, Simon M.; Mu, Linjing; European Journal of Medicinal Chemistry; vol. 92; (2015); p. 554 – 564;,
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Adding a certain compound to certain chemical reactions, such as: 112-47-0, 1,10-Decanediol, 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, Application In Synthesis of 1,10-Decanediol, blongs to alcohols-buliding-blocks compound. Application In Synthesis of 1,10-Decanediol

Hydrobromic acid (1.2 mL 48% aqueous solution, 9.5 mmol) was added to a suspension of 1,10-decanediol 1 (1.5 g, 8.6 mmol) in 30 mL of toluene in a round-bottomed flask equipped with a Dean-Stark trap and a cooler. The mixture was refluxed for 16 h. After cooling, the solvent was removed under reduced pressure. The residue obtained was chromatographed on silica gel using hexane/ethyl acetate (8:2) to yield the pure compound 2 (Scheme 1). Yield 74%; yellow oily product: IR (KBr): v = 3325, 2925, 2850,1450, 1250, 1050, 700, 625, 550 cm-1. 1H NMR (200 MHz, CDCl3): delta1.20-1.40 (m, 12H), 1.45-1.60 (m, 2H), 1.84 (qn, J=6.8 Hz, 2H), 3.39 (t, J=6.8 Hz, 2H), 3.62 (t, J=6.4 Hz, 2H) ppm. 13C NMR (50 MHz, CDCl3) delta: 25.67, 28.11, 28.69, 29, 32, 29.42, 32.73, 32.77, 33.98, 62.99 ppm.

The synthetic route of 112-47-0 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Guimaraes, Daniel Silqueira Martins; de Sousa Luz, Leticia Silveira; do Nascimento, Sara Batista; Silva, Lorena Rabelo; de Miranda Martins, Natalia Rezende; de Almeida, Heloisa Goncalves; de Souza Reis, Vitoria; Maluf, Sarah El Chamy; Budu, Alexandre; Marinho, Juliane Aparecida; Abramo, Clarice; Carmona, Adriana Karaoglanovic; da Silva, Marina Goulart; da Silva, Gisele Rodrigues; Kemmer, Victor Matheus; Butera, Anna Paola; Ribeiro-Viana, Renato Marcio; Gazarini, Marcos Leoni; Junior, Clebio Soares Nascimento; Guimaraes, Luciana; dos Santos, Fabio Vieira; de Castro, Whocely Victor; Viana, Gustavo Henrique Ribeiro; de Brito, Cristiana Ferreira Alves; de Pilla Varotti, Fernando; European Journal of Pharmaceutical Sciences; vol. 138; (2019);,
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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. 1450754-41-2, name is 2-(3-But-3-ynyl-3H-diazirin-3-yl)-ethanol, molecular formula is C7H10N2O, 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. Safety of 2-(3-But-3-ynyl-3H-diazirin-3-yl)-ethanol

(f) imidazole (740 mg, 10.87 mmol, 3.0 eq),Triphenylphosphine (1.05 g, 3.99 mmol, 1.1 eq)Add dichloromethane (5ml) to the reaction flask and cool to 0 C.Add iodine (1.1 g, 4.35 mmol, 1.2 eq),Add the insulation reaction for 30 minutes.Add compound 5 (500 mg, 3.62 mmol, 1 eq) at low temperatureA solution of methylene chloride (1 ml) was added and the reaction was kept for 4 hours.Quenched with saturated sodium sulfite solution, extracted with ethyl acetate.Dry, spin dry, and purified by column to obtain 400 mg of compound 6,Yield: 46%

With the rapid development of chemical substances, we look forward to future research findings about 1450754-41-2.

Reference:
Patent; Suzhouguangdian Biological Technology Co., Ltd.; Ni Runyan; Wang Wei; (7 pag.)CN109438211; (2019); A;,
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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. 3973-18-0, name is Propynol ethoxylate. A new synthetic method of this compound is introduced below., Quality Control of Propynol ethoxylate

Production of 2-((4-methylcyclohexa-l,4-dienyl)methoxy)ethyl 4-methylbenzenesulfonate and 2-((5 -methylcyclohexa- 1 ,4-dienyl)methoxy)ethyl 4-methylbenzenesulfonate[Chem. 24] 100.00 g (0.59 mol) of the diene alcohol obtained in Example 36, 90.29 g (0.89 mol) of Iriethylamine, and 73.20 g (0.89 mol) of 1-methylimidazole were dissolved in 400 ml of toluene. In an ice bath, a toluene solution (400 ml) of 130.33 g (0.68 mol) of p-toluenesulfonyl chloride was slowly added dropwise to the solution, and then the resulting mixture was stirred for one hour at room temperature. Water was added thereto, and the organic layer was separated. The obtained organic layer was washed sequentially with 15% sulfuric acid, water, and a saturated aqueous sodium hydrogen carbonate. The solvent was distilled off under reduced pressure, and thus 188.01 g of the desired tosylate was obtained as a colorless oil. Yield 98.1% (l,4-type/l,5-type = 91/9).1.67 (s, 3H), 2.44 (s, 3H), 2.58 (brs, 4H), 3.58 – 3.55 (m, 2H), 3.84 (s, 2H), 4.18 – 4.14 (m, 2H), 5.41 – 5.40 (m, 1H), 5.64 – 5.63 (m, 1H), 7.33 (d, J = 8.3 Hz, lH), 7.80 (d, J = 8.3 Hz, 1H);HRMS (ESI):Calculated value: [M+H]+ 323.1312Found value: 323.1325

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, 3973-18-0, Propynol ethoxylate.

Reference:
Patent; TAKASAGO INTERNATIONAL CORPORATION; TOUGE, Taichiro; NARA, Hideki; HAKAMADA, Tomohiko; WO2012/26201; (2012); A1;,
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Adding a certain compound to certain chemical reactions, such as: 86770-74-3, 2-(2-(2-(2-Aminoethoxy)ethoxy)ethoxy)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, Product Details of 86770-74-3, blongs to alcohols-buliding-blocks compound. Product Details of 86770-74-3

Example 4 This example describes two methods for the preparation of bis-N,N’-(2-(2-(2-(2-hydroxyethoxy)ethoxy)ethoxy)ethyl)perylenetetracarboxylic diimide. Method A: 2-[2-[2-(2-Aminoethoxy)ethoxy]ethoxy]ethanol (2.6 g, 13.5 mmol), perylenetetracarboxylic dianhydride (2.2 g, 5.6 mmol), and triethylamine (25 mL, 180 mmol) were mixed with 50 mL of dry DMSO (4A activated MS, 3 days) in a 250-mL flask under argon. After the reaction mixture was stirred for 4 h at 150 C., the reaction solution was cooled to 80 C. and transferred to a 1000-mL flask. A mixture of 600 mL 10% aqueous HCl and 300 mL methanol was added to the reaction solution, then the solution was stirred for additional 2 hours at 60 C. After the mixture was cooled to RT overnight, the precipitate was collected using paper filter. The resulting collection was washed with 400 mL water, and the water layer was re-extracted with 50 mL chloroform. The filtrate could be extracted with chloroform to gain more products, but these products were contaminated and needed column purification. The combined organic layer was concentrated to give the crude title product; further purification was carried out on a silica-gel column eluted with CH2Cl2/CH3OH (5:1). Detection of the products on TLC plates was accomplished using UV light or sulfuiric acid solution (5% conc. sulfuric acid in EtOH). The title compound was obtained as dark-red solid (3.6 g, 86% yield): Rf0.4 (CH2Cl2/CH3OH, 10:1). 1H-NMR (60-70 mg/0.5 ml; CDCl3/CD3OD/100/5) delta7.96 (d, 4H, J=8.1 Hz, aromatic ring), 7.61 (d, 4H, J=8.1 Hz, aromatic ring), 4.32 (t, 4H, J=5.7 Hz, CH2N), 3.65-3.29 (m, 28H, CH2OCH2, HOCH2); 13C-NMR (60-70 mg/0.5 ml; CDCl3/CD3OD/100/5) delta162.7, 133.1, 130.4, 128.1, 124.7, 122.5, 122.4, 72.9, 70.79, 70.76, 70.4, 70.2, 68.0, 61.6, 39.5. 1H-NMR (DMSO-d6) delta7.13 (bd, 4H, aromatic ring), 6.92 (bd, 4H, aromatic ring), 4.59 (t, 4H, J=5.7 Hz, CH2N), 3.65-3.29 (m, 28H, CH2OCH2, HOCH2); 13C-NMR (DMSO-d6) delta161.2, 131.4, 128.8, 125.9, 122.6, 120.2, 72.3, 69.8, 69.7, 69.6, 66.5, 60.2, 45.67. MS (MALDI): m/z 765.82 [M+Na]+. Anal. Calcd. for C40H42N2O12 (742.77): C, 64.68; H, 5.70; N, 3.77. Found: C, 64.24; H, 5.52; N, 3.83.

The synthetic route of 86770-74-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Washington State University Research Foundation; US7238792; (2007); B2;,
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Adding a certain compound to certain chemical reactions, such as: 10160-24-4, 7-Bromo-1-heptanol, 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, Computed Properties of C7H15BrO, blongs to alcohols-buliding-blocks compound. Computed Properties of C7H15BrO

2-(7-Bromoheptyloxy)tetrahydro-2H-pyran2 (3): Dihydropyran (5.20 g, 6.11 mmol) was added to a stirring 0C solution of 7-bromoheptane-l-ol (2) (1 1.0 g, 56.7 mmol) and a catalytic amount of PTSA in CH2C12. After stirring at rt for 12 h, the reaction mixture was diluted with CH2C12 (200 mL), washed with water (100 mL x 2), brine (100 mL chi 3), dried over anhydrous sodium sulphate, and evaporated. The residue was purified by silica gel column chromatography using a gradient of 10-20% ethyl acetate/hexane as eluent to give 2-(7- bromoheptyloxy)tetrahydro-2H-pyran (3) (14.50 g, 92%) as a colorless oil. TLC: 10% EtOAc/hexanes, Rf ~ 0.55; NMR (400 MHz, CDC13) delta 4.58-4.56 (m, 1H), 3.84-3.88 (m, 1H), 3.68-3.77 (m, 1H), 3.46-3.51 (m, 1H), 3.33-3.43 (m, 3H), 1.80-1.81 (m, 2H), 1.30-1.62 (m, 14 H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,10160-24-4, 7-Bromo-1-heptanol, and friends who are interested can also refer to it.

Reference:
Patent; MCW RESEARCH FOUNDATION, INC.; IMIG, John, David; CAMPBELL, William, B.; FALCK, John, Russell; WO2012/138706; (2012); A1;,
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Electric Literature of 17100-58-2, 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. 17100-58-2, name is (4-Bromo-2-methylphenyl)methanol, molecular formula is C8H9BrO, 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.

Step 2: 4-bromo-l-(bromomethyl)-2-methylbenzene; Hydrobromic acid (cone, 2 eq.) was added to a stirred solution of the alcohol from step 1 (1 eq.) in acetic acid (0.22M). The mixture was stirred at 50 C for 12 h, cooled down to room temperature, poured in water and extracted with Et2O. The organic extract was washed with water, aqueous sodium hydrogen carbonate (3x), brine, dried over MgSO4, filtered and concentrated to afford the desired benzyl bromide as a light yellow solid.

According to the analysis of related databases, 17100-58-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; MERCK FROSST CANADA LTD.; WO2009/23964; (2009); A1;,
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