Category: alcohols-buliding-blocks

Related Products of 2566-44-1, 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 2566-44-1 as follows.

Reaction A : Dissolve oxalyl chloride (9.3 mL, 106.7 mmol) in dichloromethane (140 mL) at ambient temperature, then cool to-78C and add slowly a solution of DMSO (11.22 g, 143.6 mmol) in dichloromethane (20 mL) while venting the mixture and stir the reaction at-78C for 20 minutes. Add 2-cyclopropyl-ethanol (6.11 g, 71.21 mmol) in dichloromethane (20 mL). Warm to 0C and add dichloromethane (25 mL) to assist with stirring and mix for 30 minutes. Dilute this reaction mixture with 100 mL THF and pour into a cold (-78C) solution of Reaction B. Reaction B : Add a solution of tert-butyl acetate (62 mL, 424 mmol) in THF (60 mL) to a cold solution (-78C) of lithium diisopropylamine (2M in heptanes/tetrahydrofuran/ethylbenzene, 180 mL, 360 mmol) in anhydrous THF (700 mL) and stir at-78C for 1.5-2 hours. Add crude Reaction A prepared as described above and rinse with 100 mL anhydrous THF. Stir at-78C for 1.5 hours then add water/diethyl ether and warm to ambient temperature overnight. Separate the layers and extract the aqueous layer with diethyl ether (3x). Dry the combined organic extracts over anhydrous MgS04, filter, and concentrate in vacuo. Purify the reaction on silica gel eluting with 20% EtOAc/hexanes to give 4-cyclopropyl-3-hydroxy-butyric acid tert butyl ester (10. 65 g. 75%).’H NMR (CDC13) 6 4.11-4. 05 (m, 1H), 3. 12 (d, 1H), 2.53 (dd, 1H), 2.38 (dd, 1H), 1. 60- 1.48 (m, 1H), 1.47 (s, 9H), 1.32-1. 23 (m, 1H), 0.80-0. 73 (m, 1H), 0.51-0. 46 (m, 2H), 0. 13-0. 04 (m, 2H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,2566-44-1, its application will become more common.

Reference:
Patent; ELI LILLY AND COMPANY; WO2005/92835; (2005); A1;,
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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. 530-91-6, name is 1,2,3,4-Tetrahydronaphthalen-2-ol, the common compound, a new synthetic route is introduced below. SDS of cas: 530-91-6

A solution of alcohol 13 (262 mg, 1.77 mmol, 1 eq.), nosyl chloride (781.5 mg, 3.53 mmol,2.0 eq.), DMAP (73.2 mg, 0.60 mmol, 0.34 eq.) and Et3N (0.74 mL,540.2 mg, 5.34 mmol, 3.0 eq.) in CH2Cl2 (6 mL) wasstirred vigorously for 16 h at rt. 2M NaOH (6 mL) was added and the reactionmixture was extracted with CH2Cl2 (3 x 5 mL). The organiclayer was washed with 2M NaOH (7 mL), dried (Na2SO4),filtered and concentrated in vacuo. The crude product was purified by fc (d = 3cm, l = 13 cm, v = 25 mL, cyclohexane:EtOAc 8:2, Rf = 0.55) to obtain a colorlessoil, yield 380.0 mg (64 %). C16H15NO5S (333.4g/mol). 1H NMR (400 MHz, CDCl3): delta (ppm) = 2.03 – 2.15(m, 2H, 3-CH2), 2.77 – 2.85 (m, 1H, 1-CH2), 2.92 – 3.02(m, 2H, 4-CH2), 3.08 (dd, J = 16.8/4.9 Hz, 1H, 1-CH2),5.10 – 5.15 (m, 1H, 2-CH), 6.95 (dd, J = 7.3/1.5 Hz, 1H,tetraline), 7.05 – 7.16 (m, 3H, tetraline), 8.08 – 8.14 (m, 2H, nos), 8.35 -8.40 (m, 2H, nos).

The synthetic route of 530-91-6 has been constantly updated, and we look forward to future research findings.

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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Synthetic Route of 311-86-4, 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. 311-86-4, name is 2-Bromo-3,3,3-trifluoropropan-1-ol. A new synthetic method of this compound is introduced below.

Adding a moisture content of 4000 ppm in a 50 mL stainless steel autoclave equipped with agitation3,3,3-trifluoropropylene oxide (33.6 g, 0.3 mol), 3-bromo-1,1,1-trifluoro-2-propanol (2.3 g, 12 mol),2,3-dibromo-1,1,1,2,3,3-hexafluoropropane (5.6 g, 18 mol), imidazole (1.6 g, 24 mmol),After sealing, the reactor was replaced twice with CO2, and the stirring was set to a reaction temperature of 120 C.Continuously pass CO2 to maintain the reaction pressure at 2MPa, react for 4h, cool to normal temperature, and slowly releaseTo the excess CO2 gas, 50% water of a molar amount of 3,3,3-trifluoroepoxypropane was added to the reaction solution, and the reaction was stirred at 50 C for about 24 hours to obtain 3,3,3-trifluoro. Crude product of propylene carbonate and 3,3,3-trifluoro-1,2-propanediol, analysis of reaction product distribution by gas chromatography, separation,Refined process to get the target product3,3,3-trifluoropropene carbonate and42.3 g of 3,3,3-trifluoro-1,2-propanediol was used to calculate the yield

At the same time, in my other blogs, there are other synthetic methods of this type of compound,311-86-4, 2-Bromo-3,3,3-trifluoropropan-1-ol, and friends who are interested can also refer to it.

Reference:
Patent; Xi’an Modern Chemical Institute; Lv Jian; Ma Hui; Zhang Wei; Wang Bo; Zeng Jijun; Zhao Bo; Yang Zhiqiang; Qin Yue; Bai Yanbo; Li Fengxian; (10 pag.)CN108178752; (2018); A;,
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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. 504-63-2, name is 1,3-Propanediol, molecular formula is C3H8O2, 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: 504-63-2

General procedure: To a solution of 1,3-propanediol (19) (6.51 mL, 90 mmol) in dry DMF (40 mL) was added NaH (60% oil dispersion; 1.20 g, 30 mmol) in installments at 0 C and the mixture was stirred at room temperature for 10 min. Dodecyl bromide (4.80 mL, 20 mmol) and KI (3.32 g, 20 mmol) were added and the mixture was heated at 95 C for 4 h. After cooling, the mixture was poured into ice-water and extracted with AcOEt. The extracts were washed with brine, dried over Na2SO4 and evaporated. The resulting residue was purified by flash CC (silica gel; AcOEt/hexane, 1:2) to provide dodecyl ether 20a (3.38 g, 69%). Tetradecyl ether 20b (79%) and hexadecyl ether 20c (77%) were similarly prepared from 1,3-propanediol (19).

With the rapid development of chemical substances, we look forward to future research findings about 504-63-2.

Reference:
Article; Yamano, Yumiko; Tsuboi, Kazuhito; Hozaki, Yuki; Takahashi, Kiyohiro; Jin, Xing-Hua; Ueda, Natsuo; Wada, Akimori; Bioorganic and Medicinal Chemistry; vol. 20; 11; (2012); p. 3658 – 3665;,
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Application of 62285-58-9, 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 62285-58-9, name is (2,6-Dimethylphenyl)methanol. This compound has unique chemical properties. The synthetic route is as follows.

Step B Preparation of N- (2,6-Dimethylbenzyl)phthalimide: To a stirred solution of 2,6-Dimethylbenzyl Alcohol (Step A, 6.59 g, 48.4 mmol) in DMSO (20 ml) was added chlorotrimethylsilane (15.75 ml, 145 mmol) at room temperature, and the mixture was stirred for one hr. To this reaction mixture were added ethyl acetate and water, the organic layer was washed with brine, dried over Na2SO4, filtered and concentrated to give an oil. The oily residue was redissolved in DMF (100 ml) and potassium phthalimide (10.76 g, 58.1 mmol) was added. The reaction mixture was stirred for 16 hours at room temperature, ethyl acetate was added, and the organic layer was washed with 3% Na2CO3, 1 N HCl, dried over Na2SO4, filtered and concentrated to give white solid. The purification was done by flash chromatography on silica gel column (chloroform: methanol 95:5) to provide the title compound as white solid. 1H NMR (270 MHz, DMSO): 2.3 (s, 6H); 4.8 (s, 2H); 7.0 (m, 3H); 7.8 (s, 4H).

According to the analysis of related databases, 62285-58-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Sharma, Shalini; von Borstel, Reid W.; US2003/149107; (2003); A1;,
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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. 163119-16-2, name is 2,6-Di-tert-butyl-4-methylcyclohexanol. A new synthetic method of this compound is introduced below., Application In Synthesis of 2,6-Di-tert-butyl-4-methylcyclohexanol

Synthesis of malonic acid ethyl 2,6-di-tert-butyl-4-methylcyclohexyl ester (d) Trifluoroacetic anhydride (41 ml, 0.29 mol) was added, dropwise, to a solution of the above 2,6-di-tert-butyl-4-methylcyclohexanol (d) (50.2 g, 0.22 mol) in ethyl acetate (200 ml) at 0C, and then the above malonic acid ethyl ester monopotassium salt (b) (41.6 g) was added thereto, slowly. After stirring it at room temperature for 2 hours, 200 ml of water was added thereto, and then 33 g of sodium hydrogencarbonate was added, slowly, to neutralize the reaction mixture. The organic layer was separated, washed with water once, and then with brine once; then it was dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure, to obtain crude malonic acid ethyl 2,6-di-tert-butyl-4-methylcyclohexyl ester (d) (76 g). The thus obtained crude malonic acid ethyl 2,6-di-tert-butyl-4-methylcyclohexyl ester (d) was used directly in the next step without purification.

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, 163119-16-2, 2,6-Di-tert-butyl-4-methylcyclohexanol.

Reference:
Patent; FUJI PHOTO FILM CO., LTD.; EP720981; (1996); A1;,
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Reference of 68327-04-8, 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.68327-04-8, name is (1S,2S)-2-Aminocyclopentanol hydrochloride, molecular formula is C5H12ClNO, molecular weight is 137.6079, as common compound, the synthetic route is as follows.

Boc2O (3.49 g, 15.98 mmol) was added to a solution, at 0C, of (1S,2S)-2- aminocyclopentan-1-ol-HC1 (2.0 g, 14.53 mmol) and Et3N (4.05 mL, 29.06 mmol) in methanol (20 mL) and stirred. The reaction was allowed to warm to room temperature and after overnight the reaction was concentrated and the crude was purified by column chromatography to give S 13 (2.87 g) as a white solid.

Statistics shows that 68327-04-8 is playing an increasingly important role. we look forward to future research findings about (1S,2S)-2-Aminocyclopentanol hydrochloride.

Reference:
Patent; REGENTS OF THE UNIVERSITY OF MICHIGAN; WANG, Shaomeng; AGUILAR, Angelo; ZHANG, Ke; XU, Shilin; XU, Tianfeng; BERNARD, Denzil; HUANG, Liyue; (285 pag.)WO2017/192543; (2017); 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. 29683-23-6, name is Tetrahydro-2H-thiopyran-4-ol, molecular formula is C5H10OS, 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: 29683-23-6

To a mixture of 4-methoxy-2-oxo-1,2-dihydropyridine-3-carbonitrile (1.00 g), tetrahydro-2H-thiopyran-4-ol (1.18 g), triphenylphosphine (2.62 g) and tetrahydrofuran (30 mL) was added dropwise diisopropyl azodicarboxylate (2.02 g) at room temperature under nitrogen atmosphere, and the mixture was stirred overnight at room temperature. The reaction mixture was diluted with saturated aqueous sodium hydrogen carbonate solution, and the mixture was extracted twice with ethyl acetate. The extracts were combined, washed with saturated brine, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (320 mg). MS (ESI+): [M+H]+ 250.9

With the rapid development of chemical substances, we look forward to future research findings about 29683-23-6.

Reference:
Patent; Takeda Pharmaceutical Company Limited; NAGAMIYA, Hiroyuki; YOSHIDA, Masato; SETO, Masaki; MARUI, Shogo; ODA, Tsuneo; ISHICHI, Yuji; SUZUKI, Hideo; KUSUMOTO, Tomokazu; YOGO, Takatoshi; RHIM, Chul Yun; YOON, Cheolhwan; LEE, Gil Nam; KANG, Hyun Bin; KIM, Kwang Ok; JEON, Hye Sun; EP2818473; (2014); A1;,
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Electric Literature of 558-42-9, 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.558-42-9, name is 1-Chloro-2-methyl-2-propanol, molecular formula is C4H9ClO, molecular weight is 108.5667, as common compound, the synthetic route is as follows.

Example 298 Preparation of Compound Nos. II-84 and II-84a-b (1520) To a solution of 2-(8-methyl-1,2,3,4-tetrahydro-pyrido[4,3-b]indol-5-yl)-1-pyridin-4-yl-ethanol (200 mg, 0.651 mmol) in acetonitrile (4 mL), potassium carbonate (270 mg, 1.95 mmol) and 1-chloro-2-methyl-propan-2-ol (105 mg, 0.977 mmol) were added and the reaction mixture was stirred at 100¡ã C. for 12 h. The reaction mixture was diluted with water (10 mL) and extracted with EtOAc (3¡Á20 mL). The combined organic layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue was purified by column chromatography (Neutral alumina, 1percent MeOH-DCM), to yield 1-[5-(2-hydroxy-2-pyridin-4-yl-ethyl)-8-methyl-1,3,4,5-tetrahydro-pyrido[4,3-b]indol-2-yl]-2-methyl-propan-2-ol. 1H NMR (CDCl3, freebase) delta (ppm): 8.6 (d, 2H), 7.27 (m, 2H), 7.2 (m, 2H), 7.0 (d, 1H), 5.08 (t, 1H), 4.19 (m, 2H), 3.9 (bs, 2H), 3.0-3.1 (m, 2H), 2.9 (m, 1H), 2.6 (s, 2H), 2.56 (m, 1H), 2.21 (s, 3H), 1.21 (s, 6H). Separation by chiral HPLC provides enantiomers II-84a-b.

The chemical industry reduces the impact on the environment during synthesis 558-42-9, I believe this compound will play a more active role in future production and life.

Reference:
Patent; Medivation Technologies, Inc.; PROTTER, Andrew Asher; CHAKRAVARTY, Sarvajit; JAIN, Rajendra Parasmal; GREEN, Michael John; US2015/266884; (2015); A1;,
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Application of 261723-32-4, 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 261723-32-4, name is (3-Bromo-2-fluorophenyl)methanol. This compound has unique chemical properties. The synthetic route is as follows.

Pyridinium chlorochromate (22.3 g, 103 mmol, 1.91 eq) was dissolved in DCM (140 mL) and 4 Molecular Sieves (22.3 g) were added to the solution. The reaction mixture was stirred for 30 minutes. A solution of benzyl alcohol 40 (11 g, 54 mmol, 1 eq) in DCM (140 mL) was added dropwise over the course of 5 min. The orange reaction mixture immediately turned dark brown upon addition of alcohol. After stirring for 30 min, the reaction mixture was diluted with 70% Hexane/EtOAc solution (250 mL) and filtered through a plug of silica gel (150 g). The silica gel was washed with Hexane/EtOAc (500 mL), and concentrated in vacuo to afford 9.8 g of aldehyde 41 as a white solid. Yield 70% over 2 steps.

According to the analysis of related databases, 261723-32-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Infinity Discovery, Inc.; US2008/114167; (2008); A1;,
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