Month: June 2021

Adding a certain compound to certain chemical reactions, such as: 2240-88-2, 3,3,3-Trifluoropropan-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, Product Details of 2240-88-2, blongs to alcohols-buliding-blocks compound. Product Details of 2240-88-2

Step 5; Preparation of 2-cvclopropyl-9-methyl-4-(3.3,3-trifluoropropoxy)-6,7,8,9- tetrahvdro-5H-pyrimido[4,5-d]azepine dihvdrochloride; [073] To a solution of 3,3,3-trifluoropropan-1-ol (14 mg, 0.12 mmol) in 1 ,4-dioxane (1 ml.) was added potassium tert-butoxide (58 mg, 0.52 mmol), and the resulting mixture was stirred at rt for 15 min. tert-Butyl 4-chloro-2-cyclopropyl-9-methyl-5,6,8,9-tetrahydro- 7H-pyrimido[4,5-d]azepine-7-carboxylate (35 mg, 0.10 mmol) was then added, and the mixture was heated at 80°C overnight. The reaction was cooled to rt and filtered through a pad of Celite.(R).. The filtrate was concentrated under reduced pressure, and the crude material was re-dissolved in 1 ,4-dioxane. A 4M solution of hydrochloric acid in dioxane (0.1 ml_, 0.4 mmol) was added, and the mixture was stirred for 3 h. The dioxane solvent was removed under reduced pressure, and the crude residue was triturated with ethyl acetate to afford 12 mg (29percent) of desired product.

The synthetic route of 2240-88-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BAYER PHARMACEUTICALS CORPORATION; WO2006/44762; (2006); A2;,
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Application of 14722-40-8, 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 14722-40-8 as follows.

Diol 22 (4.70 g, 19.2 mmol) was dissolved in cyclohexane (50 mL) and 48% HBr (2.4 mL, 21.2 mmol, 1.1 eq.) was added under vigorous stirring. The mixture was refluxed overnight. After cooling to r.t, saturated sodium bicarbonate solution (100 mL) was added and the phases were separated. The aqueous phase was extracted with dichloromethane (3 x 50 mL). The combined organic layers were dried over MgS04. After evaporation of the solvent the product was purified by column chromatography (silica gel, 27 chi 4 cm, cyclohexane/ethyl acetate, 4:1 ? 100% ethyl acetate) and isolated as a white solid. Yield: 3.39 g (58%). Traces of 1 ,15-dibromopentadecane were also found. 23 M.p.: 63-65 C 1H-NMR (300 MHz, CDCI3) delta [ppm]: 1 .26-1.44 (m, 23 H, 3-CH2 to 13-CH2, 1 -OH), 1 .55 (m, 2 H, 2-CH2), 1 .85 (m, 2 H, 14-CH2), 3.41 (t, 3JH,H = 6.9 Hz, 2 H, 15-CH2), 3.63 (t, 3JH,H = 6.6 HZ, 2 H, 1 -CH2). 13C-NMR (75 MHz, CDCI3) delta [ppm]: 25.9 (t, C-3), 28.3, 28.9, 29.6, 29.7, 29.8 (t, C-4 to C-13), 32.9 (t, C-14), 33.0 (t, C-2), 34.2 (t, C-15), 63.1 (t, C-1 ). Ref.: Synthesis according to C. Girlanda-Junges, F. Keyling-Bilger, G. Schmitt, B. Luu, Tetrahedron 1998, 54, 7735-7748.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,14722-40-8, its application will become more common.

Reference:
Patent; WESTFAELISCHE WILHELMS-UNIVERSITAET MUENSTER; HAUFE, Guenter; LEVKAU, Bodo; SCHAEFERS, Michael; SCHILSON, Stefani Silke; KEUL, Petra; WO2013/26765; (2013); A1;,
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Reference of 505-10-2, 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. 505-10-2, name is 3-(Methylthio)propan-1-ol, molecular formula is C4H10OS, 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 1 : Synthesis of 3-(methylsulfonyl)propan-l-ol 12-a3-(methylthio)propan-l-ol (200 g, 1900 mmol, CAS 505-10-2) was dissolved in CH2C12 (2000 mL). The mixture was cooled to 0C. Then w-CPBA 85% in water (970 g, 5700 mmol, CAS 937-14-4) was added portion wise keeping the temperature between 0 and 5C. After addition, the mixture was allowed to warm to 25C and stirred for 15 h. The mixture was filtered through a celite pad. The filtrate was purified by flash column (Eluent: petroleum ether: ethyl acetate = 3 : 1 and then ethyl acetate: methanol = 10: 1) to yield the intermediate 12-a (75 g, 29%).

According to the analysis of related databases, 505-10-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; JANSSEN R&D IRELAND; COOYMANS, Ludwig Paul; DEMIN, Samuel Dominique; HU, Lili; JONCKERS, Tim Hugo Maria; RABOISSON, Pierre Jean-Marie Bernard; TAHRI, Abdellah; VENDEVILLE, Sandrine Marie Helene; WO2012/80450; (2012); A1;,
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Electric Literature of 4415-82-1, 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. 4415-82-1, name is Cyclobutylmethanol. A new synthetic method of this compound is introduced below.

2-Cyclobutanecarbaldehyde Chemical Formula: C5HgO Exact Mass: 84.06 Molecular Weight: 84.12 To a mixture of Pyridinium chlorochromate (41.3 g, 191.6 mmol) in dichloromethane (120 mL) was added Cyclobutanemethanol (7.5 g, 87.1 mmol). The mixture was stirred for 1.5 hours then filtered through a pad of silica and rinsed with further dichloromethane (300 mL). The solvent was removed under reduced pressure to give 2-cyclobutylcarbaldehyde (10.0 g, contains residual dichloromethane) that was used without further purification.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,4415-82-1, Cyclobutylmethanol, and friends who are interested can also refer to it.

Reference:
Patent; ALKERMES PHARMA IRELAND LIMITED; BLUMBERG, Laura, Cook; DEAVER, Dan; EYERMAN, David; WO2014/190270; (2014); A1;,
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Electric Literature of 111-90-0, 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.111-90-0, name is Diethylene Glycol Monoethyl Ether, molecular formula is C6H14O3, molecular weight is 134.1736, as common compound, the synthetic route is as follows.

The procedure of Example 1 was carried out except that 219 g (1.5 mol) of adipic acid was used instead of succinic acid, to synthesize 539 g of dicarbitol adipate. OH group/COOH group=1.5, and the reaction time was 14 h. Table 1 shows measured results of the acid value, saponification value, hydroxyl value, color (APHA), viscosity, water solubility, oil solubility and feeling of use of the dicarbitol adipate

The chemical industry reduces the impact on the environment during synthesis 111-90-0, I believe this compound will play a more active role in future production and life.

Reference:
Patent; Kokyu Alcohol Kogyo Co., Ltd.; US2008/200544; (2008); A1;,
Alcohol – Wikipedia,
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Related Products of 187731-65-3, 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.187731-65-3, name is (2-Amino-4-methoxyphenyl)methanol, molecular formula is C8H11NO2, molecular weight is 153.18, as common compound, the synthetic route is as follows.

General procedure: To a solution of 1a (1.2 g, 7.61 mmol) in CH2Cl2 (20 mL) was added MnO2 (2.6 g, 30.1 mmol) and stirred at rt under an Ar atmosphere. After 23 h with stirring, the reaction mixture was filtrated and evaporated. The residue was crystallized from AcOEt to give 7a (1.0 g, 85%) as a yellow needle crystal.

The chemical industry reduces the impact on the environment during synthesis 187731-65-3, I believe this compound will play a more active role in future production and life.

Reference:
Article; Ida, Yoshihiro; Matsubara, Ayaka; Nemoto, Toru; Saito, Manabu; Hirayama, Shigeto; Fujii, Hideaki; Nagase, Hiroshi; Bioorganic and Medicinal Chemistry; vol. 20; 19; (2012); p. 5810 – 5831;,
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Related Products of 4254-29-9, 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 4254-29-9, name is 2,3-Dihydro-1H-inden-2-ol. This compound has unique chemical properties. The synthetic route is as follows.

A mixture of indan-2-ol (15, 99.7 mg, 0.74 mmol, 1 eq.), pyridinium chlorochromate (241.9 mg, 1.12 mmol, 1.5 eq.) and CH2Cl2 (3 mL) was vigorously stirred for 4 h at rt. A small amount of silica was added. Et2O (5 mL) was added and the reaction mixture was filtered under pressure. The residue was washed with Et2O. The filtrate was concentrated in vacuo. The crude product was purified by fc (d = 2 cm, l = 11 cm, v = 10 mL, cyclohexane:EtOAc 8:2, Rf = 0.11), yellow oil, yield 67.1 mg (68 %). C9H8O (132.2 g/mol). FT-IR (neat): nu (cm-1) = 2924 (C-H), 1743 (C=O), 740 and 648 (1,2-disubst. arom.). 1H NMR (400 MHz, CDCl3): delta (ppm) = 3.57 (s, 4H, 1-CH2, 3-CH2), 7.26 – 7.34 (m, 4H, Ar-H). 13C NMR (101 MHz, CD3OD): delta (ppm) = 44.2 (2C, C-1, C-3), 125.1 (2C, Cind), 127.5 (2C, Cind), 137.9 (2C, Cqind), 215.3 (1C, C=O). Exact Mass (APCI): m/z = 133.0654 (calcd. 133.0648 for C9H9O [M+H+]). Purity (HPLC, method 2) = 98.8 % (tR = 14.29 min).

According to the analysis of related databases, 4254-29-9, the application of this compound in the production field has become more and more popular.

Reference:
Article; Bechthold, Elena; Gawaskar, Sandeep; Robaa, Dina; Schepmann, Dirk; Schreiber, Julian A.; Seebohm, Guiscard; Sippl, Wolfgang; Temme, Louisa; Wuensch, Bernhard; European Journal of Medicinal Chemistry; vol. 190; (2020);,
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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. 5339-85-5, name is 2-(2-Aminophenyl)ethanol. This compound has unique chemical properties. The synthetic route is as follows. Application In Synthesis of 2-(2-Aminophenyl)ethanol

Under protection of nitrogen, 2-aminophenylethanol (1.30 g, 9.5 mmol) was dissolved in anhydrous tetrahydrofuran (100 mL), the resulting solution was slowly added dropwise to a suspension of sodium hydride (60%, 0.42 g, 10.4 mmol) in anhydrous tetrahydrofuran (20 mL), the mixture was stirred for 15 min at room temperature, and added with tert-butyldiphenylchlorosilane (2.86 g, 10.4 mmol), and stirred for 20 hrs at room temperature. The reaction system was added with water, and extracted with methyl tert-butyl ester. The extracts were combined, dried with anhydrous sodium sulfate, and concentrated under reduced pressure, to obtain a brown oil (3.75 g).

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, 5339-85-5, 2-(2-Aminophenyl)ethanol.

Reference:
Patent; SHANGHAI HUILUN LIFE SCIENCE & TECHNOLOGY CO., LTD; Cheng, Jianjun; Qin, Jihong; Ye, Bin; US2014/206679; (2014); A1;,
Alcohol – Wikipedia,
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Reference of 597-31-9, 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. 597-31-9, name is 3-Hydroxy-2,2-dimethylpropanal. A new synthetic method of this compound is introduced below.

2) Synthesis of Hydroxypivalic Acid: Add 40 ml of water to a 500 ml three-necked flask, start stirring, add 85 g of hydroxypivalaldehyde and 0.85 g of phosphotungstic acid catalyst, and then start heating. When the temperature rises to 55 C, Adding 123g of hydrogen peroxide, and adding for 2 hours; the oxidizing liquid is dehydrated under reduced pressure, filtering after dehydration to obtain the catalyst, taking out and reusing, and cooling and crystallizing the filtrate to obtain hydroxypivalic acid solution. 3) Drying: Hydroxypivalic acid solution was filtered to obtain wet products, the use of vacuum dryer for drying, temperature control at 58 , vacuum control in 0.085MPa, the final product hydroxypivalic acid, product yield of 85%.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,597-31-9, 3-Hydroxy-2,2-dimethylpropanal, and friends who are interested can also refer to it.

Reference:
Patent; Jihua Jiangcheng Chemical Industry Co., Ltd; Sun, Chengjun; Chu, Ke; (8 pag.)CN105753683; (2016); A;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Related Products of 30379-58-9, 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 30379-58-9, name is Benzyl 2-hydroxyacetate. This compound has unique chemical properties. The synthetic route is as follows.

Benzyl 2-hydroxyacetate (3.2 ml, 22.2 mmol), sodium sulfate (0.63 g, 4.4 mmol), and MeCN (34 ml) were placed in a 100 ml two-necked RBF fitted with a magnetic stirrer, a dropping funnel and a refluxing condenser. 2,2-Difluoro-2-(fluorosulfonyl)acetic acid (9.18 ml, 89 mmol) was then added with stirring at 45 0C. After addition, the mixture was further stirred for 1 h at this temperature. The reaction mixture was poured into 10% aqueous sodium carbonate and was extracted with diethyl ether, the combined extracts were washed with 10% aqueous sodium carbonate, water, brine, dried over sodium sulfate, and concentrated. The crude material was purified by column chromatography (4:1 Hexanes/EtOAc) to afford the intermediate benzyl 2-(difluoromethoxy)acetate which was dissolved in EtOAc (34 mL). N-Ethyl-N-isopropylpropan-2 -amine (0.561 ml, 3.2 mmol) was added and after degassing with nitrogen, palladium on carbon (0.680 g, 0.64 mmol) was added. The reaction was purged with hydrogen and stirred under 50 PSI of hydrogen for 24 hours. The degassed reaction was filtered through a pad of Celite and concentrate to afford the titled product as the amine salt which was used directly for subsequent reaction steps without further purification.

According to the analysis of related databases, 30379-58-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; AMGEN INC.; WO2008/147547; (2008); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts