Month: July 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. 3068-00-6, name is 1,2,4-Butanetriol, molecular formula is C4H10O3, 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: 1,2,4-Butanetriol

A mixture of compound 32 (10.6 g, 100 mmol), compound 7 (10.54 g, 20 mmol) and PTSA (0.1 eq) was heatedunder toluene reflux with Soxhlet extractor containing activated 4A molecular sieves for 3 h. Removal of solvent thencolumn purification (silica gel, 0-30% EtOAc in hexanes) gave compound 33 (11 g, 90 %) as a colorless oil. 1H NMR(400 MHz, CDCl3) delta 5.45 – 5.24 (m, 8H), 4.30 – 4.17 (m, 1H), 4.08 (dd, J = 7.8, 6.1, 1H), 3.80 (dd, J = 10.6, 5.0, 3H),3.53 (t, J = 8.0, 1H), 2.77 (t, J = 6.4, 5H), 2.29 – 2.18 (m, 1H), 2.05 (q, J = 6.7, 9H), 1.86 – 1.74 (m, 2H), 1.59 (dd, J =18.3, 9.7, 5H), 1.42 – 1.18 (m, 43H), 0.89 (t, J = 6.8, 6H). 13C NMR (101 MHz, CDCl3) delta 130.39, 130.36, 130.35, 128.14,112.80, 77.54, 77.22, 76.90, 75.74, 70.14, 61.08, 37.97, 37.50, 35.56, 31.74, 30.14, 30.13, 29.88, 29.80, 29.73, 29.57,29.53, 27.45, 27.41, 25.84, 24.20, 24.00, 22.79, 14.30

With the rapid development of chemical substances, we look forward to future research findings about 3068-00-6.

Reference:
Patent; Arbutus Biopharma Corporation; Akinc, Akin; Querbes, William; Wong, Frances; Dorkin, Joseph, Robert; Qin, Xiaojun; Cantley, William; Borodovsky, Anna; De, Soma; Manoharan, Muthiah; Jayaraman, Muthusamy; Rajeev, Kallanthottathil, G.; (109 pag.)EP3243504; (2017); A1;,
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Related Products of 616-29-5, 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.616-29-5, name is 1,3-Diaminopropan-2-ol, molecular formula is C3H10N2O, molecular weight is 90.12, as common compound, the synthetic route is as follows.

General procedure: Three di-Schiff base ligands, H2L1, H2L2 and H2L3 weresynthesized in our laboratory by standard methods [10b].Salicylaldehyde (1.05 mL, 10 mM) was mixed with respectivediammines viz. 1,3-diaminopentane (0.596 mL, 5 mM), 1,3-propanediamine (0.42 mL, 5 mM), 1,3-diaminopropan-2-ol(0.295 g, 5 mM) in methanol (20 mL) and the resulting mixtureswere refluxed for ca. 1.5 h and allowed to cool to roomtemperature. The desired yellow crystalline ligands were filteredoff from each solution, washed with methanol, and dried in avacuum desiccator containing anhydrous CaCl2.

Statistics shows that 616-29-5 is playing an increasingly important role. we look forward to future research findings about 1,3-Diaminopropan-2-ol.

Reference:
Article; Seth, Piya; Figuerola, Albert; Jover, Jesus; Ruiz, Eliseo; Ghosh, Ashutosh; Polyhedron; vol. 117; (2016); p. 57 – 63;,
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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. Recommanded Product: 83647-43-2

Compound I-2-5 (3.5 g, 19.45 mmol),Compound I-2-6 (2.61 g, 12.97 mmol),Pd(dppf)Cl2·CH2Cl2 (120 mg, 1.30 mmol) was added to a 250 mL three-neck bottle.Add toluene (19 mL) and ethanol (6.35 mL).Replace N2 three times, add NaHCO3 (19mL, 2M, 38.92mmol) for 3h at room temperature,The reaction was completely detected by TLC, the reaction system was spun dry, dissolved with ethyl acetate, washed with water, and the organic phase was dried.Column chromatography gave Compound I-2-7 in an amount of 3.1 g, yield 93.2%.

With the rapid development of chemical substances, we look forward to future research findings about 83647-43-2.

Reference:
Patent; Guangzhou Dankang Pharmaceutical Biological Co., Ltd.; Xu Yong; Lin Dang; Huang Lu; Hu Hai; (36 pag.)CN110092779; (2019); 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.14320-38-8, name is Cyclopent-3-enol, molecular formula is C5H8O, molecular weight is 84.12, as common compound, the synthetic route is as follows.SDS of cas: 14320-38-8

(1) By using 2.2 g of 3-cyclopentenol prepared according to the method described in J. Org. Chem., 25, 26-29 (1960) and 9.2 g of t-butyldiphenylsilyl chloride and by the same procedures as in (1) of the intermediate preparation example 1, there was obtained 8.15 g of 3-cyclopenten-1-yl (t-butyldiphenylsilyl) ether. Yield 97%

At the same time, in my other blogs, there are other synthetic methods of this type of compound,14320-38-8, Cyclopent-3-enol, and friends who are interested can also refer to it.

Reference:
Patent; Sumitomo Chemical Company, Limited; US5925676; (1999); A;,
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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. 64372-62-9, name is 2-Chloro-5-(trifluoromethyl)benzyl alcohol. This compound has unique chemical properties. The synthetic route is as follows. Recommanded Product: 64372-62-9

A 3 M K2CO3 solution is prepared by adding solid K2CO3 (31 g, 0.22 mol) to water (100 mL). Cooling is applied to keep the solution at 20-25 C. (2-chloro-5-(trifluoromethyl)phenyl) methanol (compound of formula 13) (17.5 g, 84 mmol), and boronic acid 5 (Scheme 3) (18.1 g, 85 mmol) are added to the K2CO3 followed by THF (100 mL) rinse. The solution is degassed by sparging with argon gas for 20 min. The catalyst, 1,1 bis(di-tert-butyiphosphino)ferrocene palladium dichloride (300 mg, 0.55 mol%) is added. The organic layer turns dark brown immediately. The biphasic mixture is aged at 35-45 C with vigorous stirring for 32 hours. The mixture is cooled to room temperature and water (150 mL) is added, followed by petroleum ether (150 mL) and the aqueous layer is removed. The organic layer was washed with water (2×200 mL) and filtered through silica gel and the solvent is removed under reduced pressure to yield brownish oil which is crystallized from heptane to give a pale white solid (28.5 g, 80%). mp 93.5-95.5 C; 1H NMR (CDCl3) delta 1.24 (d, J = 6.9 Hz, 6H), 1.95 (t, J =6.1 Hz, 1H), 3.21 (sept, J = 6.9 Hz, 1H), 3.73 (s, 3H), 4.49 (m, 2H), 6.68 (d, J =12.0 Hz, 1H), 6.99 (d, J = 8.6 Hz, 1H), 7.30 (d, J = 7.9 Hz, 1H), 7.59 (dd, J1 = 8.0 Hz, J2 =1.3 Hz, 1H), 7.86 (d, J = 0.7 Hz, 1H). The impurity (5′-ethyl-4′-fluoro-2′-methoxy-4-(trifluoromethyl)biphenyl-2-yl)methanol (~ 3 %), which is formed from 5-ethyl-4-fluoro-2-methoxyphenylboronic acid present in the starting material under the conditions described in Step 5, was detected in the product.

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, 64372-62-9, 2-Chloro-5-(trifluoromethyl)benzyl alcohol.

Reference:
Patent; LEK Pharmaceuticals d.d.; EP2468736; (2012); A1;,
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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.637031-88-0, name is 3,3-Difluorocyclobutanol, molecular formula is C4H6F2O, molecular weight is 108.09, as common compound, the synthetic route is as follows.SDS of cas: 637031-88-0

A solution of (racemic)-2′,3′,4′-trifluoro-7′-(fluoromethylsulfonyl)spiro[l,3-dioxolane-2, -indane] (13.5 mg, 0.041 mmol) and 3,3-difluoro-cyclobutanol (6.5 mu^, 0.066 mmol) in acetonitrile (1.0 mL) at 25 C was treated with potassium hydroxide (3.5 mg, 0.0600mmol) and stirred at 25 C for 1 h. Volatiles were removed by concentration under reduced pressure. The reaction mixture was poured into 20 mL of water and extracted with 3 x 20 mL EtOAc. The combined organics were rinsed with 10 mL of brine, dried with MgS04, filtered, and concentrated to dryness. The product was used without further purification. ESI (+) [M+ H4]+ m/z 432.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,637031-88-0, 3,3-Difluorocyclobutanol, and friends who are interested can also refer to it.

Reference:
Patent; PELOTON THERAPEUTICS, INC.; DIXON, Darryl, David; GRINA, Jonas; JOSEY, John, A.; RIZZI, James, P.; SCHLACHTER, Stephen, T.; WALLACE, Eli, M.; WANG, Bin; WEHN, Paul; XU, Rui; YANG, Hanbiao; (237 pag.)WO2016/144825; (2016); A1;,
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Reference of 627-30-5, Adding some certain compound to certain chemical reactions, such as: 627-30-5, name is 3-Chloropropan-1-ol,molecular formula is C3H7ClO, 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 627-30-5.

Triphenylphosphine (2.6 g, 10.1 mmol) and 3-chloropropanol (0.69 ml, 8.2 mmol) were added to a suspension of 4-chloro-7-hydroxy-6-methoxyquinazoline (1.65 g, 7. 8 mmol) in dichloromethane (100 ml) under argon. The flask was placed in a water bath at 20 C and di-tert-butyl azodicarboxylate (2.30 g, 10.1 mmol) added portion wise over a few minutes. The reaction mixture was stirred at ambient temperature for 2 hours before solvent evaporation in vacuo. Purification by flash chromatography on silica gel, eluting with ethyl acetate: petroleum ether (3: 7) yielded 4-CHLORO-7- (3-CHLOROPROPOXY)-6-METHOXYQUINAZOLINE (2.0 g, 91 % yield): H-NMR (DMSO d6) : 8.90 (s, 1H), 7.55 (s, 1H), 7.45 (s, 1H), 4.42 (m, 2H), 4.05 (s, 3H), 3.80 (m, 2H), 2.31 (m, 2H).

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. 627-30-5, 3-Chloropropan-1-ol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; WO2004/113324; (2004); A1;,
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Related Products of 13330-96-6, 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 13330-96-6 as follows.

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.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,13330-96-6, its application will become more common.

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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Synthetic Route of 349-75-7, 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. 349-75-7, name is (3-(Trifluoromethyl)phenyl)methanol, molecular formula is C8H7F3O, 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.

4,6-dimethyl-5-nitro-2-hydroxypyridine (350 mg, 2.08 mmol)Dissolved in 15 mL of dry tetrahydrofuran3-trifluoromethylbenzyl alcohol (0.44 g, 2.50 mmol) was added in the presence of nitrogen,Triphenylphosphine(1.09 g, 4.16 mmol), cooled to 0 C, and azodicarbonyl diisopropyl ester (0.84 mg, 4.16 mmol) was slowly added dropwise. After the drop is finished, the roomStir for three hours. Spin-dried tetrahydrofuran, crude using petroleum ether / ethyl acetate = 30: 1 column to obtain compound 6A, whiteColor solid (589 mg, 86% yield).

According to the analysis of related databases, 349-75-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Jiangsu Xiansheng Pharmaceutical Co., Ltd.; Chen Huanming; Liang Bo; Zhao Zhongqiang; Cao Wenjie; Li Amin; Chen Dexin; Gao Chunhua; Zhang Peng; Xu Wanmei; Chen Xuelian; Zhang Lili; (29 pag.)CN103508943; (2017); B;,
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Adding a certain compound to certain chemical reactions, such as: 2568-33-4, 3-Methylbutane-1,3-diol, 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, COA of Formula: C5H12O2, blongs to alcohols-buliding-blocks compound. COA of Formula: C5H12O2

To a solution of 3-methylbutane-1 ,3-diol (2.5 ml_) in dichloromethane (30 ml_) and pyridine (2.1 ml_) is added at 0C p-toluene-sulfonylchloride (4.6 g) in portions. The mixture is stirred for 12 hours at room temperature, diluted with dichloromethane and washed with 1 M aqueous HCI solution and brine. After drying (MgSO4) the solvent is evaporated and the product is pu rified by ch romatog raphy on s il ica gel (cyclohexane/ethyl acetate 90:10?70:30) to give the title compound. Yield : 3.2 g; Mass spectrum (ESI+): m/z = 276 [M+NH4]+.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,2568-33-4, 3-Methylbutane-1,3-diol, and friends who are interested can also refer to it.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; ECKHARDT, Matthias; FRATTINI, Sara; HAMPRECHT, Dieter; HIMMELSBACH, Frank; LANGKOPF, Elke; LINGARD, Iain; PETERS, Stefan; WAGNER, Holger; WO2013/144097; (2013); A1;,
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