Month: June 2021

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. 456-47-3, name is 3-Fluorobenzyl alcohol, molecular formula is C7H7FO, 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. SDS of cas: 456-47-3

General procedure: GeneralProcedure for the preparation of 2-Phenyl-1H-benzoimidazole (3aa): A 25mL over-dried Schlenk tube was charged with 2-nitroaniline (41.4 mg, 0.3 mmol),benzyl alcohol (97.2 mg, 0.90 mmol) and Pd(dppf)Cl2 (12.2 mg, 0.015mmol). The tube was purged with nitrogen three times. Toluene (1 mL) was addedto the sealed reaction vessel by syringe. The reaction mixture was stirred in apreheated oil bath at 160 oC for 24 h. After cooling to roomtemperature, the reaction mixture was then concentrated in vacuo, and theresidue was purified by column chromatography (silica gel, petroleumether/ ethyl acetate = 4:1) to give 3aa as a pale yellow solid (56.5 mg, 97%).

With the rapid development of chemical substances, we look forward to future research findings about 456-47-3.

Reference:
Article; Li, Xiaotong; Hu, Renhe; Tong, Yao; Pan, Qiang; Miao, Dazhuang; Han, Shiqing; Tetrahedron Letters; vol. 57; 41; (2016); p. 4645 – 4649;,
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Application of 41175-50-2, 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. 41175-50-2, name is 1,2,3,5,6,7-Hexahydropyrido[3,2,1-ij]quinolin-8-ol. A new synthetic method of this compound is introduced below.

Hydroxyjulolidine (3.7 g, 19.3 mmol) and diphenyl malonate (4.1 g, 15.9 mmol) were added into anhydrous toluene (10 mL). The mixture was heated to reflux for 4 h, and compound 2 was obtained by filtration as a straw yellow solid (3.6 g, 88%): mp 268-270C; NMR (400 MHz, DMSO): delta (ppm) 1 1.73 (s, 1H), 7.15 (s, 1H), 5.21 (s, 1H), 3.24-3.20 (m, 4H), 2.70 (s, 4H), 1.91-1.83 (m, 4H); 13C NMR (100 MHz, DMSO): delta (ppm) 166.5, 162.8, 151.0, 146.0, 119.8, 117.3, 105.3, 103.1, 85.8, 49.2, 48.7, 26.9, 21.0, 20.1, 20.0.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,41175-50-2, its application will become more common.

Reference:
Patent; MICHIGAN TECHNOLOGICAL UNIVERSITY; BI, Lanrong; WO2014/63033; (2014); A2;,
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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. 3597-91-9, name is [1,1′-Biphenyl]-4-ylmethanol, the common compound, a new synthetic route is introduced below. Formula: C13H12O

In the glove box,Mn(CO)5Br (0.005 mmol),[(E)-2-(2-(1-(2-pyridyl)ethylidene)-indenyl)pyridine] (0.006 mmol),Add 1.0 mL of toluene, stir for two hours, add 2-methylquinoline 4 (2 mmol),2 g (1 mmol), after reacting at 135 C for 48 hours, the reaction was stopped and the solvent was evaporated., column chromatography ethyl acetate / petroleum ether (1:10),The trans-disubstituted olefin derivative 3ag. The product was a white solid with a yield of 92%.

The synthetic route of 3597-91-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Qingdao University of Science and Technology; Zhang Chunyan; (19 pag.)CN108250153; (2018); A;,
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Reference of 83647-43-2 , The common heterocyclic compound, 83647-43-2, name is (3-Bromo-2-methylphenyl)methanol, molecular formula is C8H9BrO, 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.

To a fiask charged with (3-bromo-2- methylphenyl)methanol (6.0 g, 30 mmol) was added a lM TFA solution of thallium trifluoroacetate (16.2 g, 29.8 mmol). The mixture was stirred at RT oyernight. Analysis by TLC showed no starting material remaining. The solyent was remoyed under yacuum, and the residuewas pumped under high yacuum for 30 min to ensure complete remoyal 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 blaeksolution 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)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).

The synthetic route of 83647-43-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; MERCK SHARP & DOHME CORP.; PASTERNAK, Alexander; DE JESUS, Reynalda, Keh; DING, Fa-xiang; DONG, Shuzhi; FRIE, Jessica; GU, Xin; JIANG, Jinlong; SHAHRIPOUR, Aurash; PIO, Barbara; TANG, Haifeng; WALSH, Shawn; WO2014/126944; (2014); A2;,
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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. 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. Quality Control of 4-(Dimethylamino)butan-1-ol

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.

With the rapid development of chemical substances, we look forward to future research findings about 13330-96-6.

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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Reference of 115-20-8 ,Some common heterocyclic compound, 115-20-8, molecular formula is C2H3Cl3O, 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.

A solution of 38 mg (0.25 mmol) of the required alcohol is added at room temperature to a mixture of 134 mg (0.25 mmol) of acid in 30 ml of DCM, 30.8 mg (0.25 mmol) of DMAP and 49 mg (0.25 mmol) of EDCI. The mixture is stirred for 20 hours at room temperature and is then evaporated todryness. A pasty oil is obtained, which is purified by chromatography (SiO2,2/3 EtOAc/heptane) to give 127 mg (76%) of a pasty product.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,115-20-8, its application will become more common.

Reference:
Patent; MERCK PATENT GMBH; WO2006/10423; (2006); A2;,
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Application of 349-95-1, Adding some certain compound to certain chemical reactions, such as: 349-95-1, name is (4-(Trifluoromethyl)phenyl)methanol,molecular formula is C8H7F3O, 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 349-95-1.

General procedure: N-Alkylation of Amides with Alcohols; General ProcedureThe amide (100 mg, 1 equiv), alcohol (3 equiv) and (Cp*IrCl2)2 (2.5mol%) were added to a microwave reactor tube. The reaction mixturewas subjected to microwave irradiation at 160 C for 3 h. The mixture was allowed to cool to r.t. and H2O (10 mL) was added. Themixture was extracted with EtOAc (3 × 10 mL). The combined organiclayers were dried (Na2SO4) and filtered. The solvent was removedunder reduced pressure and the residue was purified usingflash silica gel chromatography with CH2Cl2-MeOH (95:5) to furnishthe N-alkylamide (Tables 2 and 3).

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. 349-95-1, (4-(Trifluoromethyl)phenyl)methanol, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Apsunde, Tushar D.; Trudell, Mark L.; Synthesis; vol. 46; 2; (2014); p. 230 – 234;,
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Electric Literature of 2516-33-8, 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. 2516-33-8, name is Cyclopropylmethanol, 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.

b) 5-Bromo-6-cyclopropylmethoxy-pyridine-2-carboxylic acid Sodium hydride (4.83 g, 0.12 mol) was added into cyclopropanemethanol (CAN 2516-33- 8, 30 g) at 0 C and the mixture was stirred at 0 C for 1 h. Then to the mixture was added methyl 5-bromo-6-chloro-pyridine-2-carboxylic acid methyl ester (3 g, 12.75 mmol). The obtained solution was heated to 90 C for 2 h. Then the mixture was evaporated to dryness, the residue was dissolved in 40 mL of water, and adjusted to pH = 4 with hydrochloric acid (3 N), and extracted with ethyl acetate (3 x 30 mL). The combined organic layer was washed with water (2 x 30 mL) and brine (2 x 50 mL) then evaporated to dryness to obtain the product as a white solid (2.5 g, 76.7%); MS (EI): m/e = 272.0 [MH+] .

According to the analysis of related databases, 2516-33-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; HOFFMANN-LA ROCHE INC.; BENDELS, Stefanie; GRETHER, Uwe; KIMBARA, Atsushi; NETTEKOVEN, Matthias; ROEVER, Stephan; ROGERS-EVANS, Mark; SCHAFFTER, Ernst; SCHULZ-GASCH, Tanja; WO2014/86806; (2014); A1;,
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Related Products of 4728-12-5 ,Some common heterocyclic compound, 4728-12-5, molecular formula is C7H14O3, 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.

[000824] To a stirred suspension of pyridinium chlorochromate ( 1.1 g) and diatomaceous earth (10 g) in dichloromethane (10 mL) was added (2,2-dimethyl- 1, 3 -dioxan-5-yl)methanol (0.5 g) as a solution in dichloromethane (3 mL) dropwise. The mixture was stirred at room temperature for 2 hours. The suspension was filtered through diatomaceous earth and washed with ethyl acetate. The crude product was filtered through silica gel and concentrated to give the title compound. NMR (501 MHz, chloroform- ) delta 9.89 (s, 1H), 4.28 – 4.17 (m, 4H), 2.42 – 2.32 (m, 1H), 1.49 (s, 3H), 1.39 (s, 3H). MS (ESI) m/e 305.9 (2M+NH4)+.

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. 4728-12-5, (2,2-Dimethyl-1,3-dioxan-5-yl)methanol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ABBVIE INC.; TAO, Zhi-Fu; DOHERTY, George; WANG, Xilu; SULLIVAN, Gerard M.; SONG, Xiaohong; KUNZER, Aaron R.; WENDT, Michael D.; MARIN, Violeta L.; FREY, Robin R.; CULLEN, Steve C.; WELCH, Dennie S.; SHEN, Xiaoqiang; BENNETT, Nathan B.; HAIGHT, Anthony R.; ACKLER, Scott L.; BOGHAERT, Erwin R.; SOUERS, Andrew J.; JUDD, Andrew S.; (623 pag.)WO2016/94509; (2016); A1;,
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Adding a certain compound to certain chemical reactions, such as: 106-28-5, (2E,6E)-3,7,11-Trimethyldodeca-2,6,10-trien-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, 106-28-5, blongs to alcohols-buliding-blocks compound. Computed Properties of C15H26O

Farnesol (10) (2.0 mL, 8 mmol) was dissolved in anhydrous DMF (80 mL) and cooled to 0 C. Collidine (6.3 mL, 48 mmol) and MsCl (1.3 mL, 16 mmol) were added to the mixture. After stirring at 0 C for 15 min, anhydrous LiCl (1.35 g, 32 mmol) was added. The reaction was stirred at 0 C for 3 h. H2O (80 mL) was added and the mixture was extracted with hexane (50 mL 3). The combined organic phases were washed with CuSO4 (sat.), NaHCO3 (sat.) and brine. The resulting solution was dried over anhydrous Na2SO4 and concentrated under reduced pressure. Compound 11 was obtained as a yellow oil and used in the next step without purification.1H NMR (300 MHz, CDCl3): d (ppm) 5.46 (1H, t, J = 8.0), 5.12-5.08 (2H, m), 4.12 (2H, d, J = 8.0), 2.23-1.98 (8H, m), 1.73 (3H, s),1.66 (3H, s), 1.61 (6H, s).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,106-28-5, its application will become more common.

Reference:
Article; Tang, Xiaoping; Demiray, Melodi; Wirth, Thomas; Allemann, Rudolf K.; Bioorganic and Medicinal Chemistry; vol. 26; 7; (2018); p. 1314 – 1319;,
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