Month: July 2021

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 6966-10-5, name is (3,4-Dimethylphenyl)methanol. This compound has unique chemical properties. The synthetic route is as follows. Product Details of 6966-10-5

General procedure: The preparation of these N-sulfinylimines was performed with 0.4 mmol (±)-sulfinamide and the 1.5 equimolar amount corresponding aromatic alcohol, L-valine(0.04 mmol), FeCl3 (0.04 mmol), 4-OH-TEMPO (0.08 mmol), toluene (2.5 mL), 4AMS (0.7000 g) were added to a 100 mL schlenk tube. Then the resulting mixture wasvigorously stirred under O2 at 60 C for 24 h. After the reaction, the residue wasfiltered off, and the solvent was removed under vacuum to give the crude product,which was purified by column chromatography on silica gel to give the pure product.

With the rapid development of chemical substances, we look forward to future research findings about 6966-10-5.

Reference:
Article; Zhang, Guofu; Xing, Yunzhe; Xu, Shengjun; Ding, Chengrong; Shan, Shang; Synlett; vol. 29; 9; (2018); p. 1232 – 1238;,
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Electric Literature of 13330-96-6, 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. 13330-96-6, name is 4-(Dimethylamino)butan-1-ol, molecular formula is C6H15NO, 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.

General procedure: To a solution of 6-substituted pyridazinone 9 (0.5 mmol) in DMF (10 mL) was added Cs2CO3 (0.55 mmol). An appropriately substituted nitro benzyl chloride (0.52 mmol) was added and the resulting mixture was stirred at 40-50 C for 3 h, the solvent was removed under reduced pressure and the residue was dissolved in EtOAc (30 mL), which was then washed with brine (3 × 10 mL). The organic layer was dried over anhydrous Na2SO4 and concentrated in vacuo. The crude product, 2-nitrobenzyl-6-substituted-pyridazin-3(2H)-one (10), was used in the next step without further purification. To a solution of 10 in 95 % ethanol (50 mL) was added acetic acid (10 mmol) followed by slow addition of iron powder (2 mmol). The resulting mixture was stirred for 5 h at 100 C. The mixture was then filtered through celite and the filter cake was washed with 95 % ethanol (3 × 15 mL). The combined ethanol filtrates were evaporated in vacuo and the residue was re-dissolved in ethyl acetate (30 mL). The organic layer was washed with brine (3 × 10 mL) and 2 M NaOH (10 mL) sequentially. The organic layer was dried over anhydrous Na2SO4, evaporated in vacuo to afford 2-aminobenzyl-6-substituted-pyridazin-3(2H)-one (11) as a yellow solid, which was used without further purification. To a stirred solution of 11 and triphosgene (1 mmol) in dry dichloromethane (5 mL) was added triethylamine (2 mmol) under nitrogen atmosphere. A solution of the corresponding alcohol (1 mmol) in dichloromethane (5 mL) was added 5-10 min later and the mixture was stirred at room temperature overnight, diluted with dichloromethane (15 mL) and washed with water (3 × 20 mL). The organic phases were separated, combined, dried over anhydrous Na2SO4 and concentrated in vacuo. The residue was purified by using column chromatography to afford the corresponding product.

According to the analysis of related databases, 13330-96-6, the application of this compound in the production field has become more and more popular.

Reference:
Article; Xing, Weiqiang; Ai, Jing; Jin, Shiyu; Shi, Zhangxing; Peng, Xia; Wang, Lang; Ji, Yinchun; Lu, Dong; Liu, Yang; Geng, Meiyu; Hu, Youhong; European Journal of Medicinal Chemistry; vol. 95; (2015); p. 302 – 312;,
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Electric Literature of 5182-44-5, 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 5182-44-5, name is 2-(3-Chlorophenyl)ethanol. This compound has unique chemical properties. The synthetic route is as follows.

2-(3-chlorophenyl)ethanol (20 g) was treated with benzyltrimethylammonium hydroxide (Triton B) (2.67 mL) and the resultant mixture was stirred in vacuo for 30 minutes. The mixture was then cooled to O0C and treated with t-butyl acrylate (17.40 g). The reaction was warmed to room temperature and stirred for 16 hours. The mixture was filtered through aluminium oxide (15 g) eluting with ether (75 mL). The collected filtrate was concentrated to give the sub-titled compound (34.40 g) as an oil. 1H NMR (CDCl3) delta 7.26-7.07 (m, 4H), 3.69-3.59 (m, 4H), 2.86-2.81 (t, 2H), 2.50-2.45 (t, 2H), 1.43 (s, 9H)

According to the analysis of related databases, 5182-44-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; WO2008/96119; (2008); A1;,
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Reference of 2919-23-5, 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. 2919-23-5, name is Cyclobutanol, molecular formula is C4H8O, 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) 5-Bromo-6-cyclobutoxy-nicotinic acid 5-Bromo-6-chloronicotinic acid (CAN 29241-62-1; 3 g, 12.7 mmol) was dissolved in DMSO (30 mL); cyclobutanol (1.19 g, 1.29 ml, 16.5 mmol) and potassium hydroxide (powder) (2.14 g, 38.1 mmol) were added and the reaction mixture was stirred at room temperature for 5 h. More cyclobutanol (0.5 mL) and KOH (1 g) was added and the reaction mixture was stirred at room temperature for another 2 days. Water (30 mL) was added and the mixture was acidified (cooling) with 5 mL 37% HCl in water (pH=2). The suspension was filtered and washed with water. The cake was dried in vacuo to obtain the title compound (3.1 g, 88.7%) as white solid; MS (ESI) 270.2 (M-H)-.

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 2919-23-5, Cyclobutanol.

Reference:
Patent; Grether, Uwe; Hebeisen, Paul; Hoffmann, Torsten; Roever, Stephan; US2012/94993; (2012); A1;,
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Adding a certain compound to certain chemical reactions, such as: 612532-52-2, 3-Amino-3-(4-fluorophenyl)propan-1-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: 3-Amino-3-(4-fluorophenyl)propan-1-ol, blongs to alcohols-buliding-blocks compound. Recommanded Product: 3-Amino-3-(4-fluorophenyl)propan-1-ol

Preparation of 3-amino-3-(4-fluorophenyl)-1-propanesulfonic acid; A solution of borane:tetrahydrofurane complex (1M, 100 mL) was added dropwise over 1 hour to a cold (0 C.) suspension of DL-3-amino-3-(4-fluorophenyl)propionoc acid (7.30 g, 39.9 mmol) in THF (40 mL). The mixture was heated to reflux for 22 hours. The mixture was then cooled to 0 C. and methanol (35 mL) was added over 15 minutes. The mixture was then heated to reflux for 30 minutes and concentrated to a thick oil. The oil was coevaporated 3 times with methanol (50 mL). The crude product was used directly in next step. The oil that was obtained in the previous step was dissolved in water and added dropwise to concentrated HBr (44 mL) The solution was heated at reflux for 18 hours. It was then concentrated to dryness (11.58 g). The solid was suspended in hot heptane/2-butanone then cooled to room temperature. Ether was added and the mixture was stirred for 30 minutes. The solid was collected by filtration and rinsed with ether (9.97 g, about 66% for two steps). The 3-bromo-1-(4-fluorophenyl)-1-propylamine hydrobromide (obtained in step 2, 32 mmol) was added to a solution of sodium sulfite (3.78 g, 30 mmol) in water (40 mL). The mixture was heated at 90 C. for 2.5 hours, and was then concentrated to a thick paste. Concentrated HCl (8 mL) was added to the paste. The resulting suspension was stirred for 20 minutes at room temperature. The solid was collected by filtration and rinsed with concentrated HCl (3×30 mL). The filtrated solid was concentrated to dryness. The solid was washed in ethanol/toluene then dried in vacuo (3.79 g). The solid was recrystallized in ethanol (25 mL) and water (6 mL). After cooling to room temperature, the solid was collected by filtration, rinsed with ethanol (2×5 mL) and dried overnight at 60 C. in a vacuum oven. The title compounds was obtained as a fine white crystalline solid, yield 2.37 g, 26% overall yield. 1H NMR 1H (500 MHz, D2O) delta 2.22-2.36 (m, 2H), 2.54-2.60 (m, 1H), 2.65-2.71(m, 1H), 4.37-4.40 (m, 1H), 7.07 (t, J=8.5 Hz, 2H), 7.26-7.31 (dd, J=8.3, 5.4 Hz, 2H); 13C (125 MHz, D2O) delta 28.82, 47.1, 53.5, 116.4 (d, J=22 Hz, 2C), 139.7 (d, J=11.6 Hz, 2C), 130.9, 163.2 (d, J=246 Hz, 2C); 19F (282 MHz, D2O) -112.9 to -113.0 (m); ES-MS 232 (M-1).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,612532-52-2, 3-Amino-3-(4-fluorophenyl)propan-1-ol, and friends who are interested can also refer to it.

Reference:
Patent; Kong, Xianqi; Wu, Xinfu; Bouzide, Abderrahim; Valade, Isabelle; Migneault, David; Bellini, Francesco; US2006/183800; (2006); A1;,
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Reference of 83647-43-2, 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 83647-43-2, name is (3-Bromo-2-methylphenyl)methanol. This compound has unique chemical properties. The synthetic route is as follows.

To a flask charged with (3-bromo-2- methylphenyl)methanol (6.0 g, 30 mmol) was added a 1M TFA solution of Thallium Trifluoroacetate (16.2 g, 29.8 mmol). The mixture was stirred at RT overnight. Analysis by TLC showed no starting material remaining. The solvent was removed under vacuum, and the residue was pumped under high vacuum for 30 min to ensure complete removal of TFA. To the residue was then added Palladium(II) Chloride (529 mg, 2.98 mmol), Lithium Chloride (2.53 g, 59.7 mmol), Magnesium Oxide (2.41 g, 59.7 mmol), and MeOH (150 mL). The reaction was flushed with CO twice, and kept under CO at room temperature. Analysis by LC showed a big product spot within 2 hours. To this solution was added ethyl acetate to precipitate the salts. The black solution was filtered through a celite pad, washed with EtOAc, adsorbed onto silica and purified by silica gel chromatography to afford title compound. 1H-NMR (500 MHz, CDC13) delta ppm 7.71 (d, J= 8.0 Hz, 1H), 7.58 (d, J= 8.0 Hz, 1H), 5.25 (s, 2H), 2.37 (s, 3H).

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 83647-43-2, (3-Bromo-2-methylphenyl)methanol.

Reference:
Patent; MERCK SHARP & DOHME CORP.; DING, Fa-Xiang; DONG, Shuzhi; FRIE, Jessica; GU, Xin; JIANG, Jinlong; PASTERNAK, Alexander; TANG, Haifeng; WU, Zhicai; YU, Yang; SUZUKI, Takao; WO2014/15495; (2014); A1;,
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Adding a certain compound to certain chemical reactions, such as: 23783-42-8, 2,5,8,11-Tetraoxatridecan-13-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, Computed Properties of C9H20O5, blongs to alcohols-buliding-blocks compound. Computed Properties of C9H20O5

Synthesis of 2,5,8,11-tetraoxatridecan-13-ol Tosylate Procedure: (JACS, 2007, 129, 13364) To a solution of 2,5,8,11-tetraoxatridecan-13-ol (7 g, 33.6 mmol) and triethylamine (4.9 ml, 35.3 mmol) in dry CH2Cl2 (100 ml), 4-toluenesulfonyl chloride (6.7 g, 35.3 mmol) and DMAP (120 mg) were added. The mixture was stirred at room temperature for 20 h. The reaction mixture was washed with 80 mL of HCl (1M) and then water. The extract was dried over anhydrous MgSO4, filtrated, and the filtrate was evaporated. The residue was used in the next step without further purification. Yield: 11.0 g (90%) NMR: 1H NMR (400 MHz, CDCl3) delta 7.75-7.64 (m, 2H), 7.31-7.26 (m, 2H), 4.16-4.06 (m, 2H), 3.62 (m 2H), 3.59-3.40 (m, 10H), 3.30 (s, 3H), 2.38 (s, 3H). 13C{1H} NMR (101 MHz, CDCl3) delta 144.75 (s), 132.90 (s), 129.77 (s), 127.8 (s), 71.82 (s), 70.60 (s), 70.48 (s), 70.47 (s), 70.41 (s), 70.39 (s), 69.23 (s), 68.55 (s), 58.90 (s), 21.53 (s).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,23783-42-8, 2,5,8,11-Tetraoxatridecan-13-ol, and friends who are interested can also refer to it.

Reference:
Patent; Bergmann, Frank; Cysewski, Robert; de Cola, Luisa; Dziadek, Sebastian; Fernandez Hernandez, Jesus Miguel; Josel, Hans-Peter; Seidel, Christoph; US2015/147750; (2015); 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. 100751-63-1, name is 6-Bromo-2-naphthylmethanol, molecular formula is C11H9BrO, 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: C11H9BrO

stirring to (6-bromonaphthalen-2-yl)methanol (18.1 g, 76.7 mmol, 1.00 eq.) at 0 CPCC (34.6 g, 92.0 mmol, 1.20 eq.) was added portionwise in DCM (300 mL).The mixture was stirred at room temperature for 16 hours and then filtered.The filtrate was concentrated in vacuo. The crude product was purified by silica gel chromatography (petroleum ether: DCM = 10-70%).6-Bromonaphthalene-2-carbaldehyde (12.8 g, a two-step yield of 68%) was obtained as a white solid.

With the rapid development of chemical substances, we look forward to future research findings about 100751-63-1.

Reference:
Patent; Huazhong University of Science and Technology; Zhu Mingqiang; Wang Yalong; Li Chong; Fan Cheng; (28 pag.)CN108530392; (2018); 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.623-04-1, name is (4-Aminophenyl)methanol, molecular formula is C7H9NO, molecular weight is 123.1525, as common compound, the synthetic route is as follows.Application In Synthesis of (4-Aminophenyl)methanol

portion of HBTU (1.6 g, 4.3 mmol) was added to a solution of Fmoc-Leu(OH) (1 g, 2.8 mmol) dissolved in 5 mL of 4% NMM in DMF and was left to stir under N2 for10 min. A portion of p-aminobenzyl alcohol (357 mg, 2.89 mmol) was then added to the reactionmixture under N2. After stirring for 5 h the reaction mixture was added to 50 mL of DCM andwashed 3 times with 50 mL of 10% LiCl in water. The organic layer was dried over sodiumsulphate and evaporated to dryness under vacuum. Flash silica-gel chromatography (3.5 %MeOH in CH2Cl2) afforded 1 as a white solid (954 mg, 69%).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,623-04-1, (4-Aminophenyl)methanol, and friends who are interested can also refer to it.

Reference:
Article; Bakthavatsalam, Subha; Franz, Katherine J.; George, Daniel J.; Wiangnak, Petpailin; Zhang, Tian; Bioorganic and medicinal chemistry letters; (2020);,
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Application of 6329-73-3, 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.6329-73-3, name is 1-(Benzo[d][1,3]dioxol-5-yl)ethanol, molecular formula is C9H10O3, molecular weight is 166.1739, as common compound, the synthetic route is as follows.

General procedure: In an oven dried Schlenk tube, were added alcohol 1 (69.0-199.5 mg, 0.5 mmol), CuI (10 mol%)and 1,10-Phenanthroline (20 mol%) and K3PO4 (2 mmol) followed by the addition of dioxane (2mL) at room temperature under open air atmosphere. The stirred reaction mixture was heated inan oil bath at 80 C for 7-48 h. Progress of the reaction was monitored by TLC till the reaction iscompleted. Then, the reaction mixture was cooled to room temperature, quenched with aqueousNH4Cl solution and then extracted with CH2Cl2 (3 10 mL). The organic layer was washed withsaturated NaCl solution, dried (Na2SO4), and filtered. Evaporation of the solvent under reducedpressure and purification of the crude material by silica gel column chromatography (petroleumether/ethyl acetate) furnished the aldehyde/ketone 2 (61-97%).

Statistics shows that 6329-73-3 is playing an increasingly important role. we look forward to future research findings about 1-(Benzo[d][1,3]dioxol-5-yl)ethanol.

Reference:
Article; Reddy, Alavala Gopi Krishna; Mahendar, Lodi; Satyanarayana, Gedu; Synthetic Communications; vol. 44; 14; (2014); p. 2076 – 2087;,
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