Category: alcohols-buliding-blocks

Electric Literature of 3513-81-3, Adding some certain compound to certain chemical reactions, such as: 3513-81-3, name is 2-Methylenepropane-1,3-diol,molecular formula is C4H8O2, 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 3513-81-3.

2-Methylene-propane-1,3-diol (2.2 g; 24.96 mmol) and dibutyltin oxide (6.85 g; 27.96 mmol) were refluxed in chloroform/methanol (100 ml 10: 1) for 24 h to obtain a clear solution. The solvent was removed under reduced pressure to give the stannoxane derivative as a white solid. Cesium fluoride (7.25 g; 47.7 mmol) was added and the mixture was dried under high vacuum. To this reaction mixture, DMF (20 ml) and benzyl bromide (3.27 ml ; 27.5 mmol) were added and the reaction mixture was stirred for 24 h at 25 °C. After that, the reaction mixture was heated at 50 °C for 1 h. The mixture is cooled to 25 °C and diluted with ethyl acetate (100 ml) and water (2 ml). The reaction mixture is stirred vigorously for 30 min and then filtered through a pad of celite to remove dibutyltin oxide. The filtrate was washed with water and then with brine, dried over Na2SO4 and the solvent was removed under reduced pressure. The crude product was purified by silica gel column chromatography eluting with 20 percent ethyl acetate/hexane to yield 2.6 g (60percent) compound 71a) as oil. 1H-NMR (CDCl3) : delta 7.36-7.28 (m, 5H), 5.20 (s, 1H), 5.15 (s, 1H), 4.51 (s, 2H), 4.19 (s, 2H), 4.10 (s, 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. 3513-81-3, 2-Methylenepropane-1,3-diol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; WO2005/92881; (2005); A1;,
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Application of 110-73-6, 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. 110-73-6, name is 2-(Ethylamino)ethanol, molecular formula is C4H11NO, 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: A mixture of compound 3a or 3b (1 mmol),benzene (50 ml), Et3N (1 ml) and morpholine (1 ml) was stirred for 5 h at80C. The solvents were evaporated in vacuo and the residues werechromatographed on a column with Al2O3 (hexane-diethyl ether, 3 :1) toafford products 8a or 8b, respectively

According to the analysis of related databases, 110-73-6, the application of this compound in the production field has become more and more popular.

Reference:
Article; Sanchez Garcia, Jessica J.; Flores-Alamo, Marcos; Chirinos Flores, Denis E.; Klimova, Elena I.; Mendeleev Communications; vol. 27; 1; (2017); p. 26 – 28;,
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Reference of 34957-73-8, 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.34957-73-8, name is Methyl 9-hydroxynonanoate, molecular formula is C10H20O3, molecular weight is 188.26, as common compound, the synthetic route is as follows.

Methyl 9-hydroxydecanoate (37.6 g, 0.2 mol) and MnO2 (17.4 g, 0.2 mol) were placed in a reaction kettle, 200 ml of ethyl acetate was added, stirring was started, 180 rpm, temperature 50 ° C, real-time monitoring The reaction was carried out, and after 8 h, it was cooled to room temperature, filtered, and the solvent was evaporated under reduced pressure to give 35.3 g of white solid product

Statistics shows that 34957-73-8 is playing an increasingly important role. we look forward to future research findings about Methyl 9-hydroxynonanoate.

Reference:
Patent; Beijing Xuyang Technology Co., Ltd.; Gao Xingdong; Du Chunhua; Pan Xiaojun; Wang Penghui; (11 pag.)CN109593045; (2019); A;,
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Adding a certain compound to certain chemical reactions, such as: 75853-18-8, 2,3-Difluorobenzyl alcohol, 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: 2,3-Difluorobenzyl alcohol, blongs to alcohols-buliding-blocks compound. Recommanded Product: 2,3-Difluorobenzyl alcohol

Solid NaH (17 mg, 0.7 mmol, 7 eq. ) was added to a stirred solution of 2, 3-difluorobenzyl alcohol (0.10 g, 0.7 mmol, 7 eq. ) in dry benzene (5 mL) at 0 °C The solution was allowed to reach RT over 15 min. The product from step (a) (45 mg, 0.1 mmol, 1 eq. ) was added as a solid and the mixture was heated to reflux for 1 h. After cooling to RT, the reaction was quenched by addition of saturated aqueous NH4C1 (1 mL). The mixture was partitioned between EtOAc (10 ML) and water (10 mL). The organic phase was separated, dried over NA2S04 and evaporated. The oily residue was purified by preparative HPLC to give the title compound as an off-white solid (4.5 mg, 11 percent yield). IH NMR (CDCl3) 8 9.80-9. 20 (br s, 1H), 7.80 (s, 1H), 7.69-7. 29 (m, 3H), 6.50 (m, 1H), 5.49 (s, 2H), 4.41 (m, 1H), 3.78 (dd, 1H), 3.64 (dd, 1H), 1. 68-1. 48 (m, 3H), 0.95 (d, 3H), 0.91 (d, 3H); MS (EST) 7N/Z 406 [M+H].

The synthetic route of 75853-18-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ASTRAZENECA AB; WO2005/33115; (2005); A1;,
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Application of 124-68-5, 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. 124-68-5, name is 2-Amino-2-methyl-1-propanol, molecular formula is C4H11NO, 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: Fe(OTf)3 (1 mol%) was added to a magnetically stirred mixture of anamine (1 mmol) and Boc2O (1 mmol) at room temperature. The mixturewas stirred until completion of the reaction (TLC), then diluted withEtOAc and washed with water. The organic layer was dried overanhydrous MgSO4, then the solvent was distillated off under vacuum toyield the highly pure N-Boc derivatives

According to the analysis of related databases, 124-68-5, the application of this compound in the production field has become more and more popular.

Reference:
Article; Feng, Chengliang; Chu, Ningning; Zhang, Shuguang; Cai, Jin; Chen, Junqing; Hu, Huayou; Ji, Min; Journal of Chemical Research; vol. 37; 12; (2013); p. 757 – 760;,
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Adding a certain compound to certain chemical reactions, such as: 2867-59-6, 3-Aminobutan-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, 2867-59-6, blongs to alcohols-buliding-blocks compound. category: alcohols-buliding-blocks

Add 250.0g of absolute ethanol and 110.5g of 4-hydroxy-2-butanone to a 1L reaction flask. 85.3g of NH3 was passed in at 10 C. The reaction solution was transferred to an autoclave, and 8.0 g of Raney nickel was added.Nitrogen and hydrogen were replaced three times, pressurized to 1.3MPa with hydrogen, the mixture was stirred at 45 C for 20 hours. GC detection of 4-hydroxy-2-butanol was less than 1.0%. The product was filtered and concentrated under reduced pressure at 45 C in a water bath. The concentrated solution was dissolved in toluene and stirred at 110 C. for 4 hours. Water was separated to obtain a lower layer. After concentrating again in a water bath at 50 C, distillation under reduced pressure of -0.9 MPa was performed, and a fraction of 80-120 C was received. The fraction was diluted with 40 g of absolute ethanol, add dropwise to a 500ml reaction bottle containing 85.2g of absolute ethanol and 65.0g of L-mandelic acid. The solution was added dropwise for 1 hour and maintained at a temperature of 55 C, and then reacted at 75 C for 20 minutes. The temperature was slowly lowered for 24 hours to 12 C, a solid was precipitated and filtered to obtain a crude filter cake. Stir the crude product with 250.8 g of isopropanol at 85 C and slowly reduce the temperature to 13 C for 3 hours. Filter again to get a crude filter cake. The above-mentioned operation of beating crystal filtration was repeated three times in total. Drying gave 80.6 g of constant weight white crystals. A 250 ml reaction tank was charged with 60.0 g of methanol, 80.6 g of white crystals, and 56.4 g of a 30% sodium methoxide methanol solution. The reaction was refluxed at 65 C for 17 hours. The temperature was lowered to 3 C and stirred for 30 minutes. Filtration at 3 C and concentration at 37 C were repeated twice to obtain 43.0 g of a colorless liquid. Distillate under reduced pressure at 125 C and receive 80-120 C fractions. Yield: 28.0%, GC: 99.9%, ee value is greater than 99.9%.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,2867-59-6, its application will become more common.

Reference:
Patent; Jiangsu Baoli Chemical Co., Ltd.; Li Yiqing; Li Zhenqi; Li Tianxin; (9 pag.)CN110668958; (2020); 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. 624-95-3, name is 3,3-Dimethylbutan-1-ol, molecular formula is C6H14O, 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. Computed Properties of C6H14O

EXAMPLE 11-Comparative Example 2; Example It represents a second reference oxidation reaction under the same conditions as for Example I using the second catalyst system reported in the same source, Tetrahedron Letters, 42 (2001) 6651-6653: 51. Omg of Mn (N03) 2H20 (0. 205mmol), 49. 5mg of Cu (N03) 2. 6H20 (0. 205mmol), 85mg TEMPO (0. 536mmol) are dissolved in glacial acetic acid (7 cc) and the solution transferred into a jacketed glass reactor. The reactor is alternately evacuated and purged with oxygen at least five times and the temperature of the catalyst solution is raised to the target value of 45C under constant stirring of 150ORPM. When the temperature reached 45C, 8200 mg of 3, 3-dimethyl-1-butanol (76. 6mmol) are injected through the septum adapter using a gas tight syringe. The recorded oxygen uptake rate is 0.016mmol 02/min and the GC analysis after 300min reaction time showed traces of the desired 3, 3-dimethyl-l-butanal. The graphical presentation of this reaction is also shown in the same Figure 01, curve 2, NS1029.

With the rapid development of chemical substances, we look forward to future research findings about 624-95-3.

Reference:
Patent; THE NUTRASWEET COMPANY; WO2005/82825; (2005); A1;,
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Synthetic Route of 4442-79-9 ,Some common heterocyclic compound, 4442-79-9, molecular formula is C8H16O, 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.

Example 81Preparation of Derivative 81 According to the Present InventionDerivative 81 having the following formula was prepared as follows. Sodium hydride (343.2 mg, 8.58 mmol, 60% dispersed oil) was slowly added to cyclohexaneethanol (1 g, 7.8 mmol) dissolved in 30 ml of dried dimethylformamide under nitrogen at room temperature while stirring. The mixture was further stirred at room temperature for 30 minutes. Then, 4-fluoro-2-(trifluoromethyl)benzaldehyde (1.2 g, 7.8 mmol) dissolved in dried dimethylformamide was added thereto over 10 minutes and stirred at room temperature for 18 hours until the initial product disappeared. Subsequently, ice water was added thereto, and the resulting mixture was extracted with ethyl acetate and water. The organic layer was washed with water several times, dried with anhydrous magnesium sulfate, filtered and solvent-evaporated. The residual oil was chromatographed on the silica gel column (hexane:ethyl acetate-20:1) to afford the intermediate, 4-(2-cyclohexylethoxy)-2-(trifluoromethyl)benzaldehyde (1.77 g, yield: 75.6%).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,4442-79-9, its application will become more common.

Reference:
Patent; Cho, Hoon; Wu, Ying; Choi, Cheol-Hee; US2011/269954; (2011); A1;,
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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 2516-33-8, name is Cyclopropylmethanol. This compound has unique chemical properties. The synthetic route is as follows. SDS of cas: 2516-33-8

Intermediate 1:Preparation of cyclopropylmethyl 2,5-dioxopyrrolidin-l-yl carbonate. added bis(2,5-dioxopyrrolidin-l -yl) carbonate (7.1 g, 27.7 mmol) and triethylamine (5.8 mL, 41.6 mmol). The reaction was stirred overnight then quenched with saturated NaHC03 (aq.) and extracted with ethyl acetate (3 chi 50 mL), dried over sodium sulfate, filtered and concentrated under reduced pressure to provide the title compound as an amber oil: NMR (300 MHz, CDC13) delta 4.16 (d, J = 7.5 Hz, 2H), 2.84 (s, 4H), 1.26 (m, 1H), 0.70-0.64 (m, 2H), 0.40-0.35 (m, 2H).

With the rapid development of chemical substances, we look forward to future research findings about 2516-33-8.

Reference:
Patent; MERCK SHARP & DOHME CORP.; EDMONDSON, Scott; GUO, Zhiqiang; GEISS, William, B.; WOOD, Harold, B.; STAMFORD, Andrew, W.; MILLER, Michael, W.; DEMONG, Duane, E.; MORRIELLO, Gregori, J.; ANAND, Rajan; COLANDREA, Vincent, J.; MACALA, Megan; MALETIC, Milana; ZHU, Cheng; ZHU, Yuping; SUN, Wanying; ZHAO, Kake; HUANG, Yong; HARRIS, Joel, M.; CHANG, Lehua; KAR, Nam Fung; HU, Zhiyong; WANG, Liping; WANG, Bowei; LIU, Ping; SZEWCZYK, Jason, W.; WO2012/138845; (2012); A1;,
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Adding a certain compound to certain chemical reactions, such as: 3513-81-3, 2-Methylenepropane-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, 3513-81-3, blongs to alcohols-buliding-blocks compound. HPLC of Formula: C4H8O2

To a solution of di-tert-butyl dicarbonate (6.6 kg) in methylene chloride (15.0 L, 15 volumes) was added 2-methylene-1,3-propanediol (1.00 kg) and phase transfer catalyst tetrabutylammonium hydrogensulfate (0.641 kg). The resulting reaction mixture was then agitated vigorously at about 15° C. while adding over a 2 hr period, 6M aqueous sodium hydroxide solution (13.2 L) and controlling the temperature between 25 to 30° C. The resulting two-phase reaction mixture was subsequently agitated for a period of 2-3 hrs at 25° C.The aqueous layer was discarded and additional phase transfer catalyst tetrabutylammonium hydrogensulfate (0.064 kg, 10percent of the initial amount), di-tert-butyl dicarbonate (0.66 kg, 10percent of the initial amount), and methylene chloride (2.0 L, 2 volumes) was added to the remaining organic reaction mixture. To the reaction mixture was also added 6M aqueous sodium hydroxide solution (1.32 L, 10percent of the initial amount) over a period of about 0.5 to 1 hr, while controlling the temperature between 25 to 30° C. The resulting two-phase reaction mixture was then agitated at about 25° C. for additional 3 to 4 hr. Allowing more than 3 hrs of agitation time is often required to complete the hydrolysis of the excess di-tert-butyl dicarbonate. The aqueous layer was discarded. The resulting organic phase was washed with water (3.x.8.0 L), diluted with EtOAc (6 L, 6 volumes), and distilled to an oil foam with quantitative yield.1H (500 MHz, CDCl3) delta 5.15, 4.98, 4.79, 4.68, 4.68, 4.33, 4.31, 3.89, 3.77, 3.67, 3.45, 3.35, 3.19, 2.88, 2.78, 2.74, 2.42, 2.17, 2.11, 2.06, 1.95, 1.72, 1.66, 1.51, 1.48, 1.43, 1.34, 1.27, 1.19, 1.19, 1.18, 1.14, 1.13, 1.11, 0.95, 0.85.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,3513-81-3, its application will become more common.

Reference:
Patent; Xu, Guoyou; Gai, Yonghua; Wang, Guoqlang; Or, Yat Sun; Wang, Zhe; US2007/207972; (2007); A1;,
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